Behavior of ceramic particles at the solid-liquid metal interface in metal matrix composites

NASA Technical Reports Server (NTRS)

Stefanescu, D. M.; Dhindaw, B. K.; Kacar, S. A.; Moitra, A.

1988-01-01

Directional solidification results were obtained in order to investigate particle behavior at the solid-liquid interface in Al-2 pct Mg (cellular interface) and Al-6.1 pct Ni (eutectic interface) alloys. It is found that particles can be entrapped in the solid if adequate solidification rates and temperature gradients are used. Model results showed critical velocity values slightly higher than those obtained experimentally.

Formation of chemically bonded ceramics with magnesium dihydrogen phosphate binder

DOEpatents

Wagh, Arun S.; Jeong, Seung-Young

2004-08-17

A new method for combining magnesium oxide, MgO, and magnesium dihydrogen phosphate to form an inexpensive compactible ceramic to stabilize very low solubility metal oxides, ashes, swarfs, and other iron or metal-based additives, to create products and waste forms which can be poured or dye cast, and to reinforce and strengthen the ceramics formed by the addition of fibers to the initial ceramic mixture.

Pumpable/injectable phosphate-bonded ceramics

DOEpatents

Singh, Dileep; Wagh, Arun S.; Perry, Lamar; Jeong, Seung-Young

2001-01-01

A pumpable ceramic composition is provided comprising an inorganic oxide, potassium phosphate, and an oxide coating material. Also provided is a method for preparing pumpable ceramic-based waste forms comprising selecting inorganic oxides based on solubility, surface area and morphology criteria; mixing the selected oxides with phosphate solution and waste to form a first mixture; combining an additive to the first mixture to create a second mixture; adding water to the second mixture to create a reactive mixture; homogenizing the reactive mixture; and allowing the reactive mixture to cure.

Porous hydroxyapatite and biphasic calcium phosphate ceramics promote ectopic osteoblast differentiation from mesenchymal stem cells

NASA Astrophysics Data System (ADS)

Zhang, Lingli; Hanagata, Nobutaka; Maeda, Megumi; Minowa, Takashi; Ikoma, Toshiyuki; Fan, Hongsong; Zhang, Xingdong

2009-04-01

Because calcium phosphate (Ca-P) ceramics have been used as bone substitutes, it is necessary to investigate what effects the ceramics have on osteoblast maturation. We prepared three types of Ca-P ceramics with different Ca-P ratios, i.e. hydroxyapatite (HA), beta-tricalcium phosphate (β-TCP), and biphasic calcium phosphate (BCP) ceramics with dense-smooth and porous structures. Comprehensive gene expression microarray analysis of mouse osteoblast-like cells cultured on these ceramics revealed that porous Ca-P ceramics considerably affected the gene expression profiles, having a higher potential for osteoblast maturation. In the in vivo study that followed, porous Ca-P ceramics were implanted into rat skeletal muscle. Sixteen weeks after the implantation, more alkaline-phosphatase-positive cells were observed in the pores of hydroxyapatite and BCP, and the expression of the osteocalcin gene (an osteoblast-specific marker) in tissue grown in pores was also higher in hydroxyapatite and BCP than in β-TCP. In the pores of any Ca-P ceramics, 16 weeks after the implantation, we detected the expressions of marker genes of the early differentiation stage of chondrocytes and the complete differentiation stage of adipocytes, which originate from mesenchymal stem cells, as well as osteoblasts. These marker gene expressions were not observed in the muscle tissue surrounding the implanted Ca-P ceramics. These observations indicate that porous hydroxyapatite and BCP had a greater potential for promoting the differentiation of mesenchymal stem cells into osteoblasts than β-TCP.

A Novel Polymer-Synthesized Ceramic Composite Based System for Bone Repair: Osteoblast Growth on Scaffolds with Varied Calcium Phosphate Content

DTIC Science & Technology

2005-01-01

demongtrated the synthesis of degradable scaffolds from PLAGA /calcium phosphate composite microspheres in which an amorphous calcium phosphate is...EXPERIMENTAL DETAILS Scaffold Preparation Scaffolds were prepared as described in detail previously [3]. Briefly, PLAGA /calcium phosphate composite...culture polystyrene (TCPS) 2- pure PLAGA microspheres 64 3- composite microsphere matrices with a low polymer/ceramic ratio 4- composite microsphere

Thermomechanical Simulation of the Splashing of Ceramic Droplets on a Rigid Substrate

NASA Astrophysics Data System (ADS)

Bertagnolli, Mauro; Marchese, Maurizio; Jacucci, Gianni; St. Doltsinis, Ioannis; Noelting, Swen

1997-05-01

Finite element simulation techniques have been applied to the spreading process of single ceramic liquid droplets impacting on a flat cold surface under plasma-spraying conditions. The goal of the present investigation is to predict the geometrical form of the splat as a function of technological process parameters, such as initial temperature and velocity, and to follow the thermal field developing in the droplet up to solidification. A non-linear finite element programming system has been utilized in order to model the complex physical phenomena involved in the present impact process. The Lagrangean description of the motion of the viscous melt in the drops, as constrained by surface tension and the developing contact with the target, has been coupled to an analysis of transient thermal phenomena accounting also for the solidification of the material. The present study refers to a parameter spectrum as from experimental data of technological relevance. The significance of process parameters for the most pronounced physical phenomena is discussed as are also the consequences of modelling. We consider the issue of solidification as well and touch on the effect of partially unmelted material.

Phosphate-bonded ceramic–wood composites : R&D project overview and invitation to participate

Treesearch

Theodore L. Laufenberg; Matt Aro

2004-01-01

We are developing chemically bonded ceramic phosphate binders for the production of biofiber-based composite materials. These binders promise to have better processing and properties than some current cement and polymer resin binder systems. The ceramic phosphate binders (termed Ceramicrete), if used in place of cement and polymers, will significantly reduce the...

Recycling of spent adsorbents for oxyanions and heavy metal ions in the production of ceramics.

PubMed

Verbinnen, Bram; Block, Chantal; Van Caneghem, Jo; Vandecasteele, Carlo

2015-11-01

Spent adsorbents for oxyanion forming elements and heavy metals are classified as hazardous materials and they are typically treated by stabilization/solidification before landfilling. The use of lime or cement for stabilization/solidification entails a high environmental impact and landfilling costs are high. This paper shows that mixing spent adsorbents in the raw material for the production of ceramic materials is a valuable alternative to stabilize oxyanion forming elements and heavy metals. The produced ceramics can be used as construction material, avoiding the high economic and environmental impact of stabilization/solidification followed by landfilling. To study the stabilization of oxyanion forming elements and heavy metals during the production process, two series of experiments were performed. In the first series of experiments, the main pollutant, Mo was adsorbed onto iron-based adsorbents, which were then mixed with industrial sludge (3 w/w%) and heated at 1100°C for 30 min. Mo was chosen, as this element is easily adsorbed onto iron-based adsorbents and it is the element that is the most difficult to stabilize (i.e. the highest temperatures need to be reached before the concentrations in the leachate are reduced). Leaching concentration from the 97/3 sludge/adsorbent mixture before heating ranged between 85 and 154 mg/kg; after the heating process they were reduced to 0.42-1.48 mg/kg. Mo was actually stabilized, as the total Mo concentration after addition was not affected by the heat treatment. In the second series of experiments, the sludge was spiked with other heavy metals and oxyanion forming elements (Cr, Ni, Cu, Zn, As, Cd and Pb) in concentrations 5 times higher than the initial concentrations; after heat treatment the leachate concentrations were below the regulatory limit values. The incorporation of spent adsorbents in ceramic materials is a valuable and sustainable alternative to the existing treatment methods, saving raw materials in the ceramics production process and avoiding the use of stabilizing agents. Besides, spent adsorbents added to the raw material for ceramic products, may improve their aesthetic and structural properties. Copyright © 2015 Elsevier Ltd. All rights reserved.

Removal of inclusions from silicon

NASA Astrophysics Data System (ADS)

Ciftja, Arjan; Engh, Thorvald Abel; Tangstad, Merete; Kvithyld, Anne; Øvrelid, Eivind Johannes

2009-11-01

The removal of inclusions from molten silicon is necessary to satisfy the purity requirements for solar grade silicon. This paper summarizes two methods that are investigated: (i) settling of the inclusions followed by subsequent directional solidification and (infiltration by ceramic foam filters. Settling of inclusions followed by directional solidification is of industrial importance for production of low-cost solar grade silicon. Filtration is reported as the most efficient method for removal of inclusions from the top-cut silicon scrap.

Preparation, mechanical property and cytocompatibility of freeze-cast porous calcium phosphate ceramics reinforced by phosphate-based glass.

PubMed

Yang, Yanqiu; He, Fupo; Ye, Jiandong

2016-12-01

In this study, phosphate-based glass (PG) was used as a sintering aid for freeze-cast porous biphasic calcium phosphate (BCP) ceramic, which was sintered under a lower temperature (1000°C). The phase composition, pore structure, compressive strength, and cytocompatibility of calcium phosphate composite ceramics (PG-BCP) were evaluated. The results indicated that PG additive reacted with calcium phosphate during the sintering process, forming β-Ca2P2O7; the ions of sodium and magnesium from PG partially substituted the calcium sites of β-calcium phosphate in BCP. The PG-BCP showed good cytocompatibility. The pore width of the porous PG-BCP ceramics was around 50μm, regardless of the amount of PG sintering aid. As the content of PG increased from 0wt.% to 15wt.%, the compressive strength of PG-BCP increased from 0.02 MP to 0.28MPa. When the PG additive was 17.5wt.%, the compressive strength of PG-BCP dramatically increased to 5.66MPa. Addition of 15wt.% PG was the critical point for the properties of PG-BCP. PG is considered as an effective sintering aid for freeze-cast porous bioceramics. Copyright © 2016 Elsevier B.V. All rights reserved.

The precursors effects on biomimetic hydroxyapatite ceramic powders.

PubMed

Yoruç, Afife Binnaz Hazar; Aydınoğlu, Aysu

2017-06-01

In this study, effects of the starting material on chemical, physical, and biological properties of biomimetic hydroxyapatite ceramic powders (BHA) were investigated. Characterization and chemical analysis of BHA powders were performed by using XRD, FT-IR, and ICP-AES. Microstructural features such as size and morphology of the resulting BHA powders were characterized by using BET, nano particle sizer, pycnometer, and SEM. Additionally, biological properties of the BHA ceramic powders were also investigated by using water-soluble tetrazolium salts test (WST-1). According to the chemical analysis of BHA ceramic powders, chemical structures of ceramics which are prepared under different conditions and by using different starting materials show differences. Ceramic powders which are produced at 80°C are mainly composed of hydroxyapatite, dental hydroxyapatite (contain Na and Mg elements in addition to Ca), and calcium phosphate sulfide. However, these structures are altered at high temperatures such as 900°C depending on the features of starting materials and form various calcium phosphate ceramics and/or their mixtures such as Na-Mg-hydroxyapatite, hydroxyapatite, Mg-Whitlockit, and chloroapatite. In vitro cytotoxicity studies showed that amorphous ceramics produced at 80°C and ceramics containing chloroapatite structure as main or secondary phases were found to be extremely cytotoxic. Furthermore, cell culture studies showed that highly crystalline pure hydroxyapatite structures were extremely cytotoxic due to their high crystallinity values. Consequently, the current study indicates that the selection of starting materials which can be used in the production of calcium phosphate ceramics is very important. It is possible to produce calcium phosphate ceramics which have sufficient biocompatibility at physiological pH values and by using appropriate starting materials. Copyright © 2017 Elsevier B.V. All rights reserved.

Thermophysical and structural studies on some glass-ceramics and role of nano size crystallites

NASA Astrophysics Data System (ADS)

Kothiyal, G. P.; Arvind, A.; Kumar, Rakesh; Dixit, Anupam; Sharma, Kuldeep; Goswami, Madhumita

2009-07-01

In this paper, we present some studies on structure and thermophysical properties of glass and glass-ceramics with possible bio-medical and sealing applications. The glass-ceramics prepared for bio-medical applications include phosphate as well as silico-phosphate compositions. In vitro bio-compatibility/activity of these materials is discussed. The glass-ceramics used for the sealing application are lithium aluminium silicate (LAS) and lithium zinc silicate (LZS). The phase formation and some aspects of thermophysical properties and sealing are discussed.

Scaffolds with a standardized macro-architecture fabricated from several calcium phosphate ceramics using an indirect rapid prototyping technique

PubMed Central

Wilson, C. E.; van Blitterswijk, C. A.; Verbout, A. J.; de Bruijn, J. D.

2010-01-01

Calcium phosphate ceramics, commonly applied as bone graft substitutes, are a natural choice of scaffolding material for bone tissue engineering. Evidence shows that the chemical composition, macroporosity and microporosity of these ceramics influences their behavior as bone graft substitutes and bone tissue engineering scaffolds but little has been done to optimize these parameters. One method of optimization is to place focus on a particular parameter by normalizing the influence, as much as possible, of confounding parameters. This is difficult to accomplish with traditional fabrication techniques. In this study we describe a design based rapid prototyping method of manufacturing scaffolds with virtually identical macroporous architectures from different calcium phosphate ceramic compositions. Beta-tricalcium phosphate, hydroxyapatite (at two sintering temperatures) and biphasic calcium phosphate scaffolds were manufactured. The macro- and micro-architectures of the scaffolds were characterized as well as the influence of the manufacturing method on the chemistries of the calcium phosphate compositions. The structural characteristics of the resulting scaffolds were remarkably similar. The manufacturing process had little influence on the composition of the materials except for the consistent but small addition of, or increase in, a beta-tricalcium phosphate phase. Among other applications, scaffolds produced by the method described provide a means of examining the influence of different calcium phosphate compositions while confidently excluding the influence of the macroporous structure of the scaffolds. PMID:21069558

Strengthening of phosphate ceramic foam by silicon carbide whiskers

NASA Technical Reports Server (NTRS)

Schetanov, B. V.; Prilepskiy, V. N.; Lapidovskaya, L. A.; Chernyak, A. I.; Romanovich, I. V.

1987-01-01

The influence of additions of SiC whiskers on the elastic modulus and flexural strength of phosphate ceramic foam is assessed. It is shown that the incorporation into the material composition of even small amounts (2.4 vol%) of SiC whiskers enhances the impact toughness and heat resistance of the ceramic foam. A 12.3 vol% of SiC whiskers leads to a more than threefold increase of the flexural strength. Strengthening of the phosphate ceramic foam is due to the fact that the whiskers hinder the propagation of matrix crack by increasing the work of matrix fracture. The whiskers reinforce only that volume of material which is occupied by solid matter, whereas they do not reinforce the pores.

Construction Material And Method

DOEpatents

Wagh, Arun S.; Antink, Allison L.

2006-02-21

A structural material of a polystyrene base and the reaction product of the polystyrene base and a solid phosphate ceramic. The ceramic is applied as a slurry which includes one or more of a metal oxide or a metal hydroxide with a source of phosphate to produce a phosphate ceramic and a poly (acrylic acid or acrylate) or combinations or salts thereof and polystyrene or MgO applied to the polystyrene base and allowed to cure so that the dried aqueous slurry chemically bonds to the polystyrene base. A method is also disclosed of applying the slurry to the polystyrene base.

Method of binding structural material

DOEpatents

Wagh, Arun S.; Antink, Allison L.

2007-12-25

A structural material of a polystyrene base and the reaction product of the polystyrene base and a solid phosphate ceramic. The ceramic is applied as a slurry which includes one or more of a metal oxide or a metal hydroxide with a source of phosphate to produce a phosphate ceramic and a poly (acrylic acid or acrylate) or combinations or salts thereof and polystyrene or MgO applied to the polystyrene base and allowed to cure so that the dried aqueous slurry chemically bonds to the polystyrene base. A method is also disclosed of applying the slurry to the polystyrene base.

The Particle Distribution in Liquid Metal with Ceramic Particles Mould Filling Process

NASA Astrophysics Data System (ADS)

Dong, Qi; Xing, Shu-ming

2017-09-01

Adding ceramic particles in the plate hammer is an effective method to increase the wear resistance of the hammer. The liquid phase method is based on the “with the flow of mixed liquid forging composite preparation of ZTA ceramic particle reinforced high chromium cast iron hammer. Preparation method for this system is using CFD simulation analysis the particles distribution of flow mixing and filling process. Taking the 30% volume fraction of ZTA ceramic composite of high chromium cast iron hammer as example, by changing the speed of liquid metal viscosity to control and make reasonable predictions of particles distribution before solidification.

Ectopic Osteoid and Bone Formation by Three Calcium-Phosphate Ceramics in Rats, Rabbits and Dogs

PubMed Central

Wang, Liao; Zhang, Bi; Bao, Chongyun; Habibovic, Pamela; Hu, Jing; Zhang, Xingdong

2014-01-01

Calcium phosphate ceramics with specific physicochemical properties have been shown to induce de novo bone formation upon ectopic implantation in a number of animal models. In this study we explored the influence of physicochemical properties as well as the animal species on material-induced ectopic bone formation. Three bioceramics were used for the study: phase-pure hydroxyapatite (HA) sintered at 1200°C and two biphasic calcium phosphate (BCP) ceramics, consisting of 60 wt.% HA and 40 wt.% TCP (β-Tricalcium phosphate), sintered at either 1100°C or 1200°C. 108 samples of each ceramic were intramuscularly implanted in dogs, rabbits, and rats for 6, 12, and 24 weeks respectively. Histological and histomorphometrical analyses illustrated that ectopic bone and/or osteoid tissue formation was most pronounced in BCP sintered at 1100°C and most limited in HA, independent of the animal model. Concerning the effect of animal species, ectopic bone formation reproducibly occurred in dogs, while in rabbits and rats, new tissue formation was mainly limited to osteoid. The results of this study confirmed that the incidence and the extent of material-induced bone formation are related to both the physicochemical properties of calcium phosphate ceramics and the animal model. PMID:25229501

[Osteogenic activity of porous calcium phosphate ceramics fabricated by rapid prototyping].

PubMed

He, Chenguang; Zhao, Li; Lin, Liulan; Gu, Huijie; Zhou, Heng; Cui, Lei

2010-07-01

Calcium phosphate bioceramics has a broad application prospect because of good biocompatibility, but porous scaffolds with complex shape can not be prepared by the traditional methods. To fabricate porous calcium phosphate ceramics by rapid prototyping and to investigate the in vitro osteogenic activities. The porous calcium phosphate ceramics was fabricated by rapid prototyping. The bone marrow mesenchymal stem cells (BMSCs) were isolated from bone marrow of Beagle canine, and the 3rd passage BMSCs were seeded onto the porous ceramics. The cell/ceramics composite cultured in osteogenic medium were taken as the experimental group (group A) and the cell/ceramics composite cultured in growth medium were taken as the control group (group B). Meanwhile, the cells seeded on the culture plate were cultured in osteogenic medium or growth medium respectively as positive control (group C) or negative control (group D). After 1, 3, and 7 days of culture, the cell proliferation and osteogenic differentiation on the porous ceramics were evaluated by DNA quantitative analysis, histochemical staining and alkaline phosphatase (ALP) activity. After DiO fluorescent dye, the cell adhesion, growth, and proliferation on the porous ceramics were also observed by confocal laser scanning microscope (CLSM). DNA quantitative analysis results showed that the number of BMSCs in all groups increased continuously with time. Plateau phase was not obvious in groups A and B, but it was clearly observed in groups C and D. The CLSM observation indicated that the activity of BMSCs was good and the cells spread extensively, showing good adhesion and proliferation on the porous calcium phosphate ceramics prepared by rapid prototyping. ALP quantitative analysis results showed that the stain of cells on the ceramics became deeper and deeper with time in groups A and B, the staining degree in group A were stronger than that in group B. There was no significant difference in the change of the ALP activity among 4 groups at the first 3 days (P > 0.05); the ALP activity increased obviously in 4 groups at 7 days, group A was significantly higher than other groups (P < 0.05) and groups C, D were significantly higher than group D (P < 0.05). The porous calcium phosphate ceramics has good cytocompatibility and the designed pores are favorable for cell ingrowth. The porous ceramics fabricated by rapid prototyping has prominent osteogenic differentiation activity and can be used as a choice of scaffolds for bone tissue engineering.

Containerless Liquid-Phase Processing of Ceramic Materials

NASA Technical Reports Server (NTRS)

Weber, J. K. Richard (Principal Investigator); Nordine, Paul C.

1996-01-01

The present project builds on the results of research supported under a previous NASA grant to investigate containerless liquid-phase processing of molten ceramic materials. The research used an aero-acoustic levitator in combination with cw CO2 laser beam heating to achieve containerless melting, superheating, undercooling, and solidification of poorly-conducting solids and liquids. Experiments were performed on aluminum oxide, binary aluminum oxide-silicon dioxide materials, and oxide superconductors.

EVALUATION OF CHEMICALLY BONDED PHOSPHATE CERAMICS FOR MERCURY STABILIZATION OF A MIXED SYNTHETIC WASTE

EPA Science Inventory

This experimental study was conducted to evaluate the stabilization and encapsulation technique developed by Argonne National Laboratory, called the Chemically Bonded Phosphate Ceramics technology for Hg- and HgCl₂-contaminated synthetic waste materials. Leachability ...

Recovery and safer disposal of phosphate coating sludge by solidification/stabilization.

PubMed

Ucaroglu, Selnur; Talinli, Ilhan

2012-08-30

Solidification/stabilization (S/S) of automotive phosphate coating sludge (PS) containing potentially toxic heavy metals was studied. The hazardous characteristics of this waste were assessed according to both Turkish and U.S. Environmental Protection Agency (EPA) regulations for hazardous solid waste. Unconfined compressive strength (UCS) and leaching behavior tests of the solidified/stabilized product were performed. Solidification studies were conducted using Portland cement (PC) as the binder. UCS was found to decrease with increasing waste content. It was found that recovery of the waste for construction applications was possible when the waste content of the mortar was 20% and below, but solidification for safe disposal was achieved only when higher waste concentrations were added. Cu, Cr, Ni, Pb and Zn were found to be significantly immobilized by the solidification/stabilization process. Ni and Zn, which were present at particularly high concentrations (2.281 and 135.318 g/kg respectively) in the PS, had highest the retention levels (94.87% and 98.74%, respectively) in the PC mortars. The organic contaminants and heavy metals present in PS were determined to be immobilized by the S/S process in accordance with the BS 6920 standard. Thus, the potential for hazardous PS waste to adversely impact human health and the environment was effectively eliminated by the S/S procedure. We conclude that S/S-treated PS is safe for disposal in landfills, while recovery of S/S-treated PS constituents remains possible. Copyright © 2012 Elsevier Ltd. All rights reserved.

[In vitro drug release behavior of carrier made of porous glass ceramics].

PubMed

Wang, De-ping; Huang, Wen-hai; Zhou, Nai

2002-09-01

To conduct the in vitro test on drug release of rifampin encapsulated in a carrier made of porous phosphate glass ceramics and to analyze main factors which affect the drug release rate. A certain quantitative of rifampin was sealed in a hollow cylindrical capsule which consisted of chopped calcium phosphate crystal fiber obtained from glass crystallization. The rifampin concentration was measured in the simulated physiological solution in which the capsule soaked. Rifampin could be released in a constant rate from the porous glass ceramic carrier in a long time. The release rate was dependent on the size of crystal fiber and the wall thickness of the capsule. This kind of calcium phosphate glass ceramics can be a candidate of the carrier materials used as long term drug therapy after osteotomy surgery.

The materials processing research base of the Materials Processing Center

NASA Technical Reports Server (NTRS)

Flemings, M. C.; Bowen, H. K.; Kenney, G. B.

1980-01-01

The goals and activities of the center are discussed. The center activities encompass all engineering materials including metals, ceramics, polymers, electronic materials, composites, superconductors, and thin films. Processes include crystallization, solidification, nucleation, and polymer synthesis.

Incorporation of RANKL promotes osteoclast formation and osteoclast activity on β-TCP ceramics.

PubMed

Choy, John; Albers, Christoph E; Siebenrock, Klaus A; Dolder, Silvia; Hofstetter, Wilhelm; Klenke, Frank M

2014-12-01

β-Tricalcium phosphate (β-TCP) ceramics are approved for the repair of osseous defects. In large defects, however, the substitution of the material by authentic bone is inadequate to provide sufficient long-term mechanical stability. We aimed to develop composites of β-TCP ceramics and receptor activator of nuclear factor κ-B ligand (RANKL) to enhance the formation of osteoclasts and promote cell mediated calcium phosphate resorption. RANKL was adsorbed superficially onto β-TCP ceramics or incorporated into a crystalline layer of calcium phosphate by the use of a co-precipitation technique. Murine osteoclast precursors were seeded onto the ceramics. After 15 days, the formation of osteoclasts was quantified cytologically and colorimetrically with tartrate-resistant acidic phosphatase (TRAP) staining and TRAP activity measurements, respectively. Additionally, the expression of transcripts encoding the osteoclast gene products cathepsin K, calcitonin receptor, and of the sodium/hydrogen exchanger NHA2 were quantified by real-time PCR. The activity of newly formed osteoclasts was evaluated by means of a calcium phosphate resorption assay. Superficially adsorbed RANKL did not induce the formation of osteoclasts on β-TCP ceramics. When co-precipitated onto β-TCP ceramics RANKL supported the formation of mature osteoclasts. The development of osteoclast lineage cells was further confirmed by the increased expression of cathepsin K, calcitonin receptor, and NHA2. Incorporated RANKL stimulated the cells to resorb crystalline calcium phosphate. Our in vitro study shows that RANKL incorporated into β-TCP ceramics induces the formation of active, resorbing osteoclasts on the material surface. Once formed, osteoclasts mediate the release of RANKL thereby perpetuating their differentiation and activation. In vivo, the stimulation of osteoclast-mediated resorption may contribute to a coordinated sequence of material resorption and bone formation. Further in vivo studies are needed to confirm the current in vitro findings. Copyright © 2014 Elsevier Inc. All rights reserved.

Property measurements and solidification studies by electrostatic levitation.

PubMed

Paradis, Paul-François; Yu, Jianding; Ishikawa, Takehiko; Yoda, Shinichi

2004-11-01

The National Space Development Agency of Japan has recently developed several electrostatic levitation furnaces and implemented new techniques and procedures for property measurement, solidification studies, and atomic structure research. In addition to the contamination-free environment for undercooled and liquid metals and semiconductors, the newly developed facilities possess the unique capabilities of handling ceramics and high vapor pressure materials, reducing processing time, and imaging high luminosity samples. These are exemplified in this paper with the successful processing of BaTiO(3). This allowed measurement of the density of high temperature solid, liquid, and undercooled phases. Furthermore, the material resulting from containerless solidification consisted of micrometer-size particles and a glass-like phase exhibiting a giant dielectric constant exceeding 100,000.

Bench-Scale Evaluation Of Chemically Bonded Phosphate Ceramic Technology To Stabilize Mercury Waste Mixtures

EPA Science Inventory

This bench-scale study was conducted to evaluate the stabilization of mercury (Hg) and mercuric chloride-containing surrogate test materials by the chemically bonded phosphate ceramics technology. This study was performed as part of a U.S. EPA program to evaluate treatment and d...

The stability mechanisms of an injectable calcium phosphate ceramic suspension

PubMed Central

Fatimi, Ahmed; Tassin, Jean-François; Axelos, Monique A. V.; Weiss, Pierre

2010-01-01

Calcium phosphate ceramics are widely used as bone substitutes in dentistry and orthopedic applications. For minimally invasive surgery an injectable calcium phosphate ceramic suspension (ICPCS) was developed. It consists in a biopolymer (hydroxypropylmethylcellulose: HPMC) as matrix and bioactive calcium phosphate ceramics (biphasic calcium phosphate: BCP) as fillers. The stability of the suspension is essential to this generation of “ready to use” injectable biomaterial. But, during storage, the particles settle down. The engineering sciences have long been interested in models describing the settling (or sedimentation) of particles in viscous fluids. Our work is dedicated to the comprehension of the effect of the formulation on the stability of calcium phosphate suspension before and after steam sterilization. The rheological characterization revealed the macromolecular behavior of the suspending medium. The investigations of settling kinetics showed the influence of the BCP particle size and the HPMC concentration on the settling velocity and sediment compactness before and after sterilization. To decrease the sedimentation process, the granule size has to be smaller and the polymer concentration has to increase. A much lower sedimentation velocity, as compared to Stokes law, is observed and interpreted in terms of interactions between the polymer network in solution and the particles. This experimentation highlights the granules spacer property of hydrophilic macromolecules that is a key issue for interconnection control, one of the better ways to improve osteoconduction and bioactivity. PMID:20229185

The stability mechanisms of an injectable calcium phosphate ceramic suspension.

PubMed

Fatimi, Ahmed; Tassin, Jean-François; Axelos, Monique A V; Weiss, Pierre

2010-06-01

Calcium phosphate ceramics are widely used as bone substitutes in dentistry and orthopedic applications. For minimally invasive surgery an injectable calcium phosphate ceramic suspension (ICPCS) was developed. It consists in a biopolymer (hydroxypropylmethylcellulose: HPMC) as matrix and bioactive calcium phosphate ceramics (biphasic calcium phosphate: BCP) as fillers. The stability of the suspension is essential to this generation of "ready to use" injectable biomaterial. But, during storage, the particles settle down. The engineering sciences have long been interested in models describing the settling (or sedimentation) of particles in viscous fluids. Our work is dedicated to the comprehension of the effect of the formulation on the stability of calcium phosphate suspension before and after steam sterilization. The rheological characterization revealed the macromolecular behavior of the suspending medium. The investigations of settling kinetics showed the influence of the BCP particle size and the HPMC concentration on the settling velocity and sediment compactness before and after sterilization. To decrease the sedimentation process, the granule size has to be smaller and the polymer concentration has to increase. A much lower sedimentation velocity, as compared to Stokes law, is observed and interpreted in terms of interactions between the polymer network in solution and the particles. This experimentation highlights the granules spacer property of hydrophilic macromolecules that is a key issue for interconnection control, one of the better ways to improve osteoconduction and bioactivity.

Directionally Solidified Multifunctional Ceramics

DTIC Science & Technology

2006-12-01

Vidrio , Vol. 44 [5] (2005) pp 347 - 352. 9. F. W. Dynys and A. Sayir, "Self Assemble Silicide Architectures by Directional Solidification," Journal...Sociedad Espanola de Ceramica y Vidrio , Vol. 43 [4] (2004) pp 753 - 758. 21. A. Sayir and F. S. Lowery, "Combustion-Resistance of Silicon-Based Ceramics...Espafiola de Cerdmica y Vidrio , Vol. 43 [3], 2004. ISSN-0366-3175-BSCVB9. 14 37. P. Berger, A. Sayir and M. H. Berger, "Nuclear Microprobe using Elastic

Influence of strontium on the synthesis and surface properties of biphasic calcium phosphate (BCP) bioceramics.

PubMed

Kanchana, Ponnusamy; Sekar, Chinnathambi

2010-01-01

Biphasic calcium phosphate (BCP) ceramics are suitable for synthetic bone applications. The strontium substituted calcium phosphate ceramics have potential for use in orthopedic surgeries. Aim of the present work is to introduce strontium into BCP (composed of hydroxyapatite and tricalcium phosphate) ceramics and to study their bioactivity and mechanical properties. BCP ceramics have been synthesized at room temperature under the physiological pH of 7.4 by gel method in the presence of strontium (5, 10 M %). The appropriate choice of anhydrous CaCl₂ as precursor solution has promoted the formation of BCP instead of pure HA for CaCl₂.2H₂O. Powder X-ray diffraction analysis confirmed the formation of BCP with different HA and ß -TCP ratios depending upon the Sr content. The presence of Sr has reduced the nucleation and growth rate of BCP when compared to pure system. The SEM micrographs showed that the microstructural morphology of BCP changes from fibrous to platelet. Nanoindentation studies indicate a significant decrease in the hardness and elastic modulus values of BCP ceramics due to Sr doping. In vitro bioactivity study has revealed the formation of apatite layer on the Sr doped BCP samples and the doping enhanced its bioactivity.

Synthesis, characterization and bioactivity of a calcium-phosphate glass-ceramics obtained by the sol-gel processing method.

PubMed

Jmal, Nouha; Bouaziz, Jamel

2017-02-01

In this work, a calcium-phosphate glass-ceramics was successfully obtained by heat treatment of a mixture of 26.52 in wt.% of fluorapatite (Fap) and 73.48 in wt.% of 77S (77 SiO 2 14 CaO9 P 2 O 5 in wt.%) gel. The calcium phosphate-glass-ceramics was prepared by sol-gel process with tetraethyl orthosilicate (TEOS), triethyl phosphate (TEP), calcium nitrate and fluorapatite. The synthesized powders were characterized by some commonly used tools such as X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), 31 P magic angle spinning nuclear magnetic resonance (MAS-NMR), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), and thin-film X-ray diffraction (TF-XRD). The obtained results seemed to confirm the nucleation and growth of hydroxyapatite (Hap) nano-phase in the glass. Moreover, an in-vitro evaluation of the glass-ceramic was performed. In addition, to assess its bioactive capacity, it was soaked in simulated body fluid (SBF) at different time intervals. The SEM, EDS and TF-XRD analyses showed the deposition of hydroxyapatite on the surface of the specimens after three days of immersion in SBF solution. The mechanical properties of the obtained material such as rupture strength, Vickers hardness and elastic modulus were measured. In addition, the friction coefficient of calcium phosphate-glass-ceramics was tested. The values of the composite of rupture strength (24MPa), Vickers hardness (214Hv), Young's modulus (52.3GPa), shear modulus (19GPa) and friction coefficient (0.327) were obtained. This glass-ceramics can have useful applications in dental prostheses. Indeed, this material may have promising applications for implants because of its content of fluorine, the effective protector against dental caries. Copyright © 2016 Elsevier B.V. All rights reserved.

Chemically bonded phospho-silicate ceramics

DOEpatents

Wagh, Arun S.; Jeong, Seung Y.; Lohan, Dirk; Elizabeth, Anne

2003-01-01

A chemically bonded phospho-silicate ceramic formed by chemically reacting a monovalent alkali metal phosphate (or ammonium hydrogen phosphate) and a sparsely soluble oxide, with a sparsely soluble silicate in an aqueous solution. The monovalent alkali metal phosphate (or ammonium hydrogen phosphate) and sparsely soluble oxide are both in powder form and combined in a stochiometric molar ratio range of (0.5-1.5):1 to form a binder powder. Similarly, the sparsely soluble silicate is also in powder form and mixed with the binder powder to form a mixture. Water is added to the mixture to form a slurry. The water comprises 50% by weight of the powder mixture in said slurry. The slurry is allowed to harden. The resulting chemically bonded phospho-silicate ceramic exhibits high flexural strength, high compression strength, low porosity and permeability to water, has a definable and bio-compatible chemical composition, and is readily and easily colored to almost any desired shade or hue.

Iron-phosphate ceramics for solidification of mixed low-level waste

DOEpatents

Aloy, Albert S.; Kovarskaya, Elena N.; Koltsova, Tatiana I.; Macheret, Yevgeny; Medvedev, Pavel G.; Todd, Terry

2000-01-01

A method of immobilizing mixed low-level waste is provided which uses low cost materials and has a relatively long hardening period. The method includes: forming a mixture of iron oxide powders having ratios, in mass %, of FeO:Fe.sub.2 O.sub.3 :Fe.sub.3 O.sub.4 equal to 25-40:40-10:35-50, or weighing a definite amount of magnetite powder. Metallurgical cinder can also be used as the source of iron oxides. A solution of the orthophosphoric acid, or a solution of the orthophosphoric acid and ferric oxide, is formed and a powder phase of low-level waste and the mixture of iron oxide powders or cinder (or magnetite powder) is also formed. The acid solution is mixed with the powder phase to form a slurry with the ratio of components (mass %) of waste:iron oxide powders or magnetite:acid solution=30-60:15-10:55-30. The slurry is blended to form a homogeneous mixture which is cured at room temperature to form the final product.

Removal of phosphorus by the core-shell bio-ceramic/Zn-layered double hydroxides (LDHs) composites for municipal wastewater treatment in constructed rapid infiltration system.

PubMed

Zhang, Xiangling; Guo, Lu; Huang, Hualing; Jiang, Yinghe; Li, Meng; Leng, Yujie

2016-06-01

Constructed rapid infiltration systems (CRIS) are a reasonable option for treating wastewater, owing to their simplicity, low cost and low energy consumption. Layered double hydroxides (LDHs), novel materials with high surface area and anion exchange capacity, faced the problem of the application in CRIS due to the powdered form. To overcome this shortcoming, Zn-LDHs (FeZn-LDHs, CoZn-LDHs, AlZn-LDHs) were prepared by co-precipitation method and in-situ coated on the surface of the natural bio-ceramic to synthesize the core-shell bio-ceramic/Zn-LDHs composites. Characterization by Scanning Electron Microscope (SEM) and X-ray Fluorescence Spectrometer (XRFS) indicated that the Zn-LDHs were successful loaded on the natural bio-ceramic. Column tests experiments indicated that the bio-ceramic/Zn-LDHs efficiently enhanced the removal performance of phosphorus. The efficiently removal rates of bio-ceramic/FeZn-LDHs were 71.58% for total phosphorous (TP), 74.91% for total dissolved phosphorous (TDP), 82.31% for soluble reactive phosphorous (SRP) and 67.58% for particulate phosphorus (PP). Compared with the natural bio-ceramic, the average removal rates were enhanced by 32.20% (TP), 41.33% (TDP), 49.06% (SRP) and 10.50% (PP), respectively. Adsorption data of phosphate were better described by the Freundlich model for the bio-ceramic/Zn-LDHs and natural bio-ceramic, except for the bio-ceramic/CoZn-LDHs. The maximum adsorption capacity of bio-ceramic/AlZn-LDHs (769.23 mg/kg) was 1.77 times of the natural bio-ceramic (434.78 mg/kg). The effective desorption of phosphate could achieve by using a mixed solution of 5 M NaCl + 0.1 M NaOH, it outperformed the natural bio-ceramic of 18.95% for FeZn-LDHs, 7.59% for CoZn-LDHs and 12.66% for AlZn-LDHs. The kinetic data of the bio-ceramic/Zn-LDHs were better described by the pseudo-second-order equation. Compared the removal amount of phosphate by the natural bio-ceramic, the physical effects were improved little, but the chemical effects were enhanced for 112.49% for FeZn-LDHs, 111.89% for CoZn-LDHs and 122.67% for AlZn-LDHs. Therefore, the way of coating Zn-LDHs on the bio-ceramic efficiently improved the chemical effects in phosphate removal, supporting that it can use as potential substrates for the removal of phosphorus in CRIS. Copyright © 2016 Elsevier Ltd. All rights reserved.

Integrated System of Thermal/Dimensional Analysis for Quality Control of Metallic Melt and Ductile Iron Casting Solidification

NASA Astrophysics Data System (ADS)

Stan, Stelian; Chisamera, Mihai; Riposan, Iulian; Neacsu, Loredana; Cojocaru, Ana Maria; Stan, Iuliana

2018-03-01

The main objective of the present work is to introduce a specific experimental instrument and technique for simultaneously evaluating cooling curves and expansion or contraction of cast metals during solidification. Contraction/expansion analysis illustrates the solidification parameters progression, according to the molten cast iron characteristics, which are dependent on the melting procedure and applied metallurgical treatments, mold media rigidity and thermal behavior [heat transfer parameters]. The first part of the paper summarizes the performance of this two-mold device. Its function is illustrated by representative shrinkage tendency results in ductile cast iron as affected by mold rigidity (green sand and furan resin sand molds) and inoculant type (FeSi-based alloys), published in part previously. The second part of the paper illustrates an application of this equipment adapted for commercial foundry use. It conducts thermal analysis and volume change measurements in a single ceramic cup so that mold media as well as solidification conditions are constants, with cast iron quality as the variable. Experiments compared gray and ductile cast iron solidification patterns. Gray iron castings are characterized by higher undercooling at the beginning and at the end of solidification and lower graphitic expansion. Typically, ductile cast iron exhibits higher graphitic, initial expansion, conducive for shrinkage formation in soft molds.

A new iron calcium phosphate material to improve the osteoconductive properties of a biodegradable ceramic: a study in rabbit calvaria.

PubMed

Manchón, Angel; Hamdan Alkhraisat, Mohammad; Rueda-Rodriguez, Carmen; Prados-Frutos, Juan Carlos; Torres, Jesús; Lucas-Aparicio, Julia; Ewald, Andrea; Gbureck, Uwe; López-Cabarcos, Enrique

2015-10-20

β-tricalcium phosphate (β-TCP) is an osteoconductive and biodegradable material used in bone regeneration procedures, while iron has been suggested as a tool to improve the biological performance of calcium phosphate-based materials. However, the mechanisms of interaction between these materials and human cells are not fully understood. In order to clarify this relationship, we have studied the iron role in β-TCP ceramics. Iron-containing β-TCPs were prepared by replacing CaCO3 with C6H5FeO7 at different molar ratios. X-ray diffraction analysis indicated the occurrence of β-TCP as the sole phase in the pure β-TCP and iron-containing ceramics. The incorporation of iron ions in the β-TCP lattice decreased the specific surface area as the pore size was shifted toward meso- and/or macropores. Furthermore, the human osteoblastlike cell line MG-63 was cultured onto the ceramics to determine cell proliferation and viability, and it was observed that the iron-β-TCP ceramics have better cytocompatibility than pure β-TCP. Finally, in vivo assays were performed using rabbit calvaria as a bone model. The scaffolds were implanted for 8 and 12 weeks in the defects created in the skullcap with pure β-TCP as the control. The in vivo behavior, in terms of new bone formed, degradation, and residual graft material were investigated using sequential histological evaluations and histomorphometric analysis. The in vivo implantation of the ceramics showed enhanced bone tissue formation and scaffold degradation for iron-β-TCPs. Thus, iron appears to be a useful tool to enhance the osteoconductive properties of calcium phosphate ceramics.

Putty-like bone fillers based on CaP ceramics or Biosilicate® combined with carboxymethylcellulose: Characterization, optimization, and evaluation.

PubMed

Gabbai-Armelin, Paulo R; Renno, Ana Cm; Crovace, Murilo C; Magri, Angela Mp; Zanotto, Edgar D; Peitl, Oscar; Leeuwenburgh, Sander Cg; Jansen, John A; van den Beucken, Jeroen Jjp

2017-08-01

Calcium phosphates and bioactive glass ceramics have been considered promising biomaterials for use in surgeries. However, their moldability should be further enhanced. We here thereby report the handling, physicochemical features, and morphological characteristics of formulations consisting of carboxymethylcellulose-glycerol and hydroxyapatite-tricalcium phosphate or Biosilicate® particles. We hypothesized that combining either material with carboxymethylcellulose-glycerol would improve handling properties, retaining their bioactivity. In addition to scanning electron microscopy, cohesion, mineralization, pH, and viscoelastic properties of the novel formulations, cell culture experiments were performed to evaluate the cytotoxicity and cell proliferation. Putty-like formulations were obtained with improved cohesion and moldability. Remarkably, mineralization in simulated body fluid of hydroxyapatite-tricalcium phosphate/carboxymethylcellulose-glycerol formulations was enhanced compared to pure hydroxyapatite-tricalcium phosphate. Cell experiments showed that all formulations were noncytotoxic and that HA-TCP60 and BGC50 extracts led to an increased cell proliferation. We conclude that combining carboxymethylcellulose-glycerol with either hydroxyapatite-tricalcium phosphate or Biosilicate® allows for the generation of moldable putties, improves handling properties, and retains the ceramic bioactivity.

Bioactive calcium phosphate-based glasses and ceramics and their biomedical applications: A review.

PubMed

Islam, Md Towhidul; Felfel, Reda M; Abou Neel, Ensanya A; Grant, David M; Ahmed, Ifty; Hossain, Kazi M Zakir

2017-01-01

An overview of the formation of calcium phosphate under in vitro environment on the surface of a range of bioactive materials (e.g. from silicate, borate, and phosphate glasses, glass-ceramics, bioceramics to metals) based on recent literature is presented in this review. The mechanism of bone-like calcium phosphate (i.e. hydroxyapatite) formation and the test protocols that are either already in use or currently being investigated for the evaluation of the bioactivity of biomaterials are discussed. This review also highlights the effect of chemical composition and surface charge of materials, types of medium (e.g. simulated body fluid, phosphate-buffered saline and cell culture medium) and test parameters on their bioactivity performance. Finally, a brief summary of the biomedical applications of these newly formed calcium phosphate (either in the form of amorphous or apatite) is presented.

Construction material

DOEpatents

Wagh, Arun S [Orland Park, IL; Antink, Allison L [Bolingbrook, IL

2008-07-22

A structural material of a polystyrene base and the reaction product of the polystyrene base and a solid phosphate ceramic is applied as a slurry which includes one or more of a metal oxide or a metal hydroxide with a source of phosphate to produce a phosphate ceramic and a poly (acrylic acid or acrylate) or combinations or salts thereof and polystyrene or MgO applied to the polystyrene base and allowed to cure so that the dried aqueous slurry chemically bonds to the polystyrene base. A method is also disclosed of applying the slurry to the polystyrene base.

Clinical Application of Ceramics in Anterior Cervical Discectomy and Fusion: A Review and Update.

PubMed

Zadegan, Shayan Abdollah; Abedi, Aidin; Jazayeri, Seyed Behnam; Bonaki, Hirbod Nasiri; Vaccaro, Alexander R; Rahimi-Movaghar, Vafa

2017-06-01

Narrative review. Anterior cervical discectomy and fusion (ACDF) is a reliable procedure, commonly used for cervical degenerative disc disease. For interbody fusions, autograft was the gold standard for decades; however, limited availability and donor site morbidities have led to a constant search for new materials. Clinically, it has been shown that calcium phosphate ceramics, including hydroxyapatite (HA) and tricalcium phosphate (TCP), are effective as osteoconductive materials and bone grafts. In this review, we present the current findings regarding the use of ceramics in ACDF. A review of the relevant literature examining the clinical use of ceramics in anterior cervical discectomy and fusion procedures was conducted using PubMed, OVID and Cochrane. HA, coralline HA, sandwiched HA, TCP, and biphasic calcium phosphate ceramics were used in combination with osteoinductive materials such as bone marrow aspirate and various cages composed of poly-ether-ether-ketone (PEEK), fiber carbon, and titanium. Stand-alone ceramic spacers have been associated with fracture and cracks. Metallic cages such as titanium endure the risk of subsidence and migration. PEEK cages in combination with ceramics were shown to be a suitable substitute for autograft. None of the discussed options has demonstrated clear superiority over others, although direct comparisons are often difficult due to discrepancies in data collection and study methodologies. Future randomized clinical trials are warranted before definitive conclusions can be drawn.

Spectroscopic properties of Eu3+/Nd3+ co-doped phosphate glasses and opaque glass-ceramics

NASA Astrophysics Data System (ADS)

Narro-García, R.; Desirena, H.; López-Luke, T.; Guerrero-Contreras, J.; Jayasankar, C. K.; Quintero-Torres, R.; De la Rosa, E.

2015-08-01

This paper reports the fabrication and characterization of Eu3+/Nd3+ co-doped phosphate (PNE) glasses and glass-ceramics as a function of Eu3+ concentration. The precursor glasses were prepared by the conventional melt quenching technique and the opaque glass-ceramics were obtained by heating the precursor glasses at 450 °C for 30 h. The structural and optical properties of the glass and glass-ceramics were analyzed by means of X-ray diffraction, Raman spectroscopy, UV-VIS-IR absorption spectroscopy, photoluminescence spectra and lifetimes. The amorphous and crystalline structures of the precursor glass and opaque glass-ceramic were confirmed by X-ray diffraction respectively. The Raman spectra showed that the maximum phonon energy decreased from 1317 cm-1 to 1277 cm-1 with the thermal treatment. The luminescence spectra of the glass and glass-ceramic samples were studied under 396 nm and 806 nm excitation. The emission intensity of the bands observed in opaque glass-ceramic is stronger than that of the precursor glass. The luminescence spectra show strong dependence on the Eu3+ ion concentration in the Nd3+ ion photoluminescence (PL) intensity, which suggest the presence of energy transfer (ET) and cross-relaxation (CR) processes. The lifetimes of the 4F3/2 state of Nd3+ ion in Eu3+/Nd3+ co-doped phosphate glasses and glass-ceramics under 806 nm excitation were measured. It was observed that the lifetimes of the 4F3/2 level of Nd3+ of both glasses and glass-ceramics decrease with the increasing Eu3+ concentration. However in the case of opaque glass-ceramics the lifetimes decrease only 16%.

Silicon on Ceramic Process: Silicon Sheet Growth and Device Development for the Large-area Silicon Sheet and Cell Development Tasks of the Low-cost Solar Array Project

NASA Technical Reports Server (NTRS)

Chapman, P. W.; Zook, J. D.; Heaps, J. D.; Pickering, C.; Grung, B. L.; Koepke, B.; Schuldt, S. B.

1979-01-01

The technical and economic feasibility of producing solar cell quality sheet silicon was investigated. It was hoped this could be done by coating one surface of carbonized ceramic substrates with a thin layer of large-grain polycrystalline silicon from the melt. Work was directed towards the solution of unique cell processing/design problems encountered with the silicon-ceramic (SOC) material due to its intimate contact with the ceramic substrate. Significant progress was demonstrated in the following areas; (1) the continuous coater succeeded in producing small-area coatings exhibiting unidirectional solidification and substatial grain size; (2) dip coater succeeded in producing thick (more than 500 micron) dendritic layers at coating speeds of 0.2-0.3 cm/sec; and (3) a standard for producing total area SOC solar cells using slotted ceramic substrates was developed.

Porous ceramics mimicking nature—preparation and properties of microstructures with unidirectionally oriented pores

PubMed Central

Okada, Kiyoshi; Isobe, Toshihiro; Katsumata, Ken-ichi; Kameshima, Yoshikazu; Nakajima, Akira; MacKenzie, Kenneth J D

2011-01-01

Porous ceramics with unidirectionally oriented pores have been prepared by various methods such as anodic oxidation, templating using wood, unidirectional solidification, extrusion, etc. The templating method directly replicates the porous microstructure of wood to prepare porous ceramics, whereas the extrusion method mimics the microstructures of tracheids and xylems in trees. These two methods are therefore the main focus of this review as they provide good examples of the preparation of functional porous ceramics with properties replicating nature. The well-oriented cylindrical through-hole pores prepared by the extrusion method using fibers as the pore formers provide excellent permeability together with high mechanical strength. Examples of applications of these porous ceramics are given, including their excellent capillary lift of over 1 m height which could be used to counteract urban heat island phenomena, and other interesting properties arising from anisotropic unidirectional porous structures. PMID:27877451

Bioactive calcium pyrophosphate glasses and glass-ceramics.

PubMed

Kasuga, Toshihiro

2005-01-01

Calcium phosphate glass-based materials in the pyrophosphate region are briefly reviewed. Calcium pyrophosphate glasses can be prepared by including a small amount of TiO(2) (

[The effects of surface morphology of calcium phosphate ceramics on apatite formation in dynamic SBF].

PubMed

Duan, Yourong; Lü, Wanxin; Wang, Chaoyuan; Chen, Jiyong; Zhang, Xingdong

2002-06-01

Bone-like apatite formation on the surface of calcium phosphate ceramics has been believed to be the prerequisite of new bone growth on ceramics and to be related to the osteoinductivity of the material. The research of the factors effecting bone-like apatite formation is a great help in understanding the mechanism of osteoinduction. This paper is aimed to a comparative study of in vitro formation of bone-like apatite on the surface of dense and rough calcium phosphate ceramics with SBF flowing at different rates. The results showed that the rough surface was beneficial to the formation of bone-like apatite, and the apatite formed faster in 1.5 SBF than in SBF. Rough surface, namely, larger surface area, increased the dissolution of Ca2+ and HPO4(2-) and higher concentration of Ca2+ and HPO4(2-) ions of SBF and was in turn advantageous to the accumulation of Ca2+, HPO4(2-), PO4(3-) near the ceramic surface. Local supersaturating concentration of Ca2+, HPO4(2-), PO4(3-) near sample surface was essential to nucleation of apatite on the surface of sample.

In vitro bioactivity behavior of modified multicomponent borate glasses containing dopants of Ag2O, CuO, CeO2 or V2O5

NASA Astrophysics Data System (ADS)

Marzouk, M. A.; ElBatal, F. H.; Ghoneim, N. A.

2018-02-01

Some multi-component borate glasses containing dopants of Ag2O, CuO, CeO2 or V2O5 were prepared. Multi-characterization techniques were carried out to investigate their bioactivity, corrosion weight loss after immersion in phosphate solution. Controlled thermal heat-treatment by two-step technique was done to convert the prepared glasses to their corresponding glass-ceramic derivatives. X-ray diffraction analysis was performed to identify the crystalline phases formed by thermal treatment. Infrared absorption of glasses and glass-ceramics reveal vibrational bands due to combined main triangular and tetrahedral borate groups in their specific wavenumbers besides some sharing of phosphate group. After immersion in the phosphate solution, two extra characteristic peaks are generated indicating the bioactivity of the studied glasses and glass-ceramics through the formation of calcium phosphate (hydroxyapatite). X-ray diffraction data indicate the formation of crystalline phases which are variable with the introduced dopants. The main crystalline phase identified is calcium borate together with some other phases some of which contain phosphate ions. These data indicate that the presence of CaO and P2O5 initiates phase separation and subsequent crystallization of the parent and doped glasses. Weight loss data indicate that glass-ceramics are obviously durable than the parent glasses. SEM micrographs of glass-ceramics before immersion show multiconstituent crystalline phases due to the basic chemical composition consisting of multicomponent mixed alkali and alkaline earth oxides beside P2O5 and with the main B2O3 constituent. After immersion, the crystalline phases are identified to be more distinct in different shapes because of the multi-composition involved.

Synthesis of β-tricalcium phosphate.

PubMed

Chaair, H; Labjar, H; Britel, O

2017-09-01

Ceramics play a key role in several biomedical applications. One of them is bone grafting, which is used for treating bone defects caused by injuries or osteoporosis. Calcium-phosphate based ceramic are preferred as bone graft biomaterials in hard tissue surgery because their chemical composition is close to the composition of human bone. They also have a marked bioresorbability and bioactivity. In this work, we have developed methods for synthesis of β-tricalcium phosphate apatite (β-TCP). These products were characterized by different techniques such as X-ray diffraction, infrared spectroscopy, scanning electron microscopy and chemical analysis. Copyright © 2017 Elsevier Masson SAS. All rights reserved.

Solid composite electrolytes for lithium batteries

DOEpatents

Kumar, Binod; Scanlon, Jr., Lawrence G.

2000-01-01

Solid composite electrolytes are provided for use in lithium batteries which exhibit moderate to high ionic conductivity at ambient temperatures and low activation energies. In one embodiment, a ceramic-ceramic composite electrolyte is provided containing lithium nitride and lithium phosphate. The ceramic-ceramic composite is also preferably annealed and exhibits an activation energy of about 0.1 eV.

[A study of bone-like apatite formation on calcium phosphate ceramics in different kinds of animals in vivo].

PubMed

Duan, Yourong; Wu, Yao; Wang, Chaoyuan; Chen, Jiyong; Zhang, Xingdong

2003-03-01

Bone-like apatite formation on the surface of calcium phosphate ceramics has been believed to be necessary for new bone to grow on the ceramics and to be related to the osteoinductivity of the material. The research of bone-like apatite formation is a great help to understanding the mechanism of osteoinduction. Synthetic porous calcium phosphate ceramics (HA/TCP = 70/30) were implanted intramuscularly in pigs, dogs, rabbits and rats to make a comparative study of the bone-like apatite formation onto the porous HA/TCP ceramics in different animals. Specimens were harvested at 14 days after implantation. Samples were detected for the surface morphology with SEM. The chemical composition of the sample surface after implantation was analyzed with reflection infrared (R-IR). Obvious bone-like apatite formation could be detected in the sections of porous specimens harvested from all animals after 14 days intramuscular implantation. Crystal deposition could be only observed on the surface of the concave regions of the samples collected from dogs, rabbits and rat. On the contrary, evenly distributed flake-shaped crystal could be found on the pore surface and also on the outer surface of the materials implanted in pigs. The morphology of bone-like apatite in pigs was different from that in the others animals. Bone-like apatite was not observed in dense specimen implanted intramuscularly. Bone-like apatite formed faster on specimens implanted in rabbit than that in other animals. This formation sequence is different from the sequence of osteoinductivity of biphasic calcium phosphate ceramics implanted in these animals. The results demonstrated that the formation of bone-like apatite on materials is a prerequisite condition to their osteoinduction but other factors also play important roles in osteoinduction.

SPS-RS technique for solid-phase “in situ” synthesis of biocompatible ZrO2 porous ceramics

NASA Astrophysics Data System (ADS)

Shichalin, O. O.; Medkov, M. A.; Grishchenko, D. N.; Mayorov, V. Yu; Fedorets, A. N.; Belov, A. A.; Golub, A. V.; Gridasova, E. A.; Papynov, E. K.

2018-02-01

The prospective method of spark plasma sintering-reaction synthesis (SPS-RS) for fabrication of ceramics based on ZrO2 and biocompatible with living tissue is presented. Nanostructured ceramics has high mechanical strength (more than 400 MPa) and controlled porosity depending on specified sintering conditions. Biocompatible phases Ca10(PO4)6(OH)2 are formed “in situ” during SPS sintering of ZrO2 powder due to chemical interaction of phosphate precursors preliminary introduced into the mixture. The effective method to improve (to develop) porous structure of bioceramics obtained by SPS or SPS-RS techniques using poreforming agent (carbon black) is proposed. Suggested original SPS-RS “in situ” technique provides fabrication of new ZrO2 ceramics containing biocompatible phosphate components and possessing unique structural and mechanical characteristics. Such ceramics is indispensable for bone-ceramic implants that are able to activate processes of osteogenesis during bone tissue recovery.

Bone morphogenetic protein Smads signaling in mesenchymal stem cells affected by osteoinductive calcium phosphate ceramics.

PubMed

Tang, Zhurong; Wang, Zhe; Qing, Fangzhu; Ni, Yilu; Fan, Yujiang; Tan, Yanfei; Zhang, Xingdong

2015-03-01

Porous calcium phosphate ceramics (CaP ceramics) could induce ectopic bone formation which was regulated by various signal molecules. In this work, bone marrow mesenchymal stem cells (MSCs) were cultured on the surface of osteoinductive hydroxyapatite (HA) and biphasic calcium phosphate (BCP) ceramics in comparison with control (culture plate) for up to 14 days to detect the signal molecules which might be affected by the CaP ceramics. Without adding osteogenic factors, MSCs cultured on HA and BCP both expressed higher Runx2, Osterix, collagen type I, osteopontin, bone sialoprotein, and osteocalcin at various stages compared with control, thus confirmed the osteoblastic differentiation of MSCs. Later study demonstrated the messenger RNA level of bone morphogenetic protein 2 (BMP2) and BMP4 were also significantly enhanced by HA and BCP. Furthermore, Smad1, 4, 5, and Dlx5, the main molecules in the BMP/Smads signaling pathway, were upregulated by HA and BCP. Moreover, the higher expression of Smads and BMP2, 4 in BCP over HA, corresponded to the better performance of BCP in stimulating in vitro osteoblastic differentiation of MSCs. This was in accordance with the better osteoinductivity of BCP over HA in vivo. Altogether, these results implied that the CaP ceramics may initiate the osteoblastic differentiation of MSCs by influencing the expression of molecules in BMP/Smads pathway. © 2014 Wiley Periodicals, Inc.

Surface or internal nucleation and crystallization of glass-ceramics

NASA Astrophysics Data System (ADS)

Höland, W.; Rheinberger, V. M.; Ritzberger, C.; Apel, E.

2013-07-01

Fluoroapatite (Ca5(PO4)3F) was precipitated in glass-ceramics via internal crystallization of base glasses. The crystals grew with a needle-like morphology in the direction of the crystallographic c-axis. Two different reaction mechanisms were analyzed: precipitation via a disordered primary apatite crystals and a solid state parallel reaction to rhenanite (NaCaPO4) precipitation. In contrast to the internal nucleation used in the formation of fluoroapatite, surface crystallization was induced to precipitate a phosphate-free oxyapatite of NaY9(SiO4)6O2-type. Internal nucleation and crystallization have been shown to be a very useful tool for developing high-strength lithium disilicate (Li2Si2O5) glass-ceramics. A very controlled process was conducted to transform the lithium metasilicate glass-ceramic precursor material into the final product of the lithium disilicate glass-ceramic without the major phase of the precursor material. The combination of all these methods allowed the driving forces of the internal nucleation and crystallization mechanisms to be explained. An amorphous phosphate primary phase was discovered in the process. Nucleation started at the interface between the amorphous phosphate phase and the glass matrix. The final products of all these glass-ceramics are biomaterials for dental restoration showing special optical properties, e.g. translucence and color close to dental teeth.

[Influence of adhesion on the color of glass infiltrated alumina ceramic restorations].

PubMed

Jiang, Li; Yang, Liu; Xu, Qiang; Guan, Hong-Yu; Wan, Qian-Bing

2006-10-01

To investigate the effects of luting agent on the final color of glass infiltrated alumina ceramic restorations. 12 plate-shaped specimens with 12.5 mm in diameter and 0.5 mm thickness were fabricated from GI-II (color IG2). Vitadur alpha veneering porcelain (color A2) with 1.0 mm thickness was fired to GI- II glass/alumina composite. 12 plate-shaped background specimens simulating the metal alloy post-and-core 12.5 mm in diameter and 2 mm thickness were also made from Ni-Cr alloy. All-ceramic specimens were luted to the metal alloy by Zinc Phosphate cement, glass ionomer cement and composite resin. The color shifts of the specimens were measured by colorimeter. Luting agents had effect on the final color of restorations. The influence of composite resin was least, followed by glass ionomer cement and Zinc Phosphate cement. The color difference between with and without Zinc Phosphate cement could be identified by the eye. To reduce the effect of luting agents, composite resin is recommended to all-ceramic restorations' adhesion.

Comparative study on in vivo response of porous calcium carbonate composite ceramic and biphasic calcium phosphate ceramic.

PubMed

He, Fupo; Ren, Weiwei; Tian, Xiumei; Liu, Wei; Wu, Shanghua; Chen, Xiaoming

2016-07-01

In a previous study, robust calcium carbonate composite ceramics (CC/PG) were prepared by using phosphate-based glass (PG) as an additive, which showed good cell response. In the present study the in vivo response of porous CC/PG was compared to that of porous biphasic calcium phosphate ceramics (BCP), using a rabbit femoral critical-size grafting model. The materials degradation and bone formation processes were evaluated by general observation, X-ray radiography, micro-computed tomography, and histological examination. The results demonstrated excellent biocompatibility and osteoconductivity, and progressive degradation of CC/PG and BCP. Although the in vitro degradation rate of CC/PG was distinctly faster than that of BCP, at 4week post-implantation, the bone generation and material degradation of CC/PG were less than those of BCP. Nevertheless, at postoperative week 8, the increment of bone formation and material degradation of CC/PG was pronouncedly larger than that of BCP. These results show that CC/PG is a potential resorbable bone graft aside from the traditional synthetic ones. Copyright © 2016 Elsevier B.V. All rights reserved.

Osteoinductive ceramics as a synthetic alternative to autologous bone grafting

PubMed Central

Yuan, Huipin; Fernandes, Hugo; Habibovic, Pamela; de Boer, Jan; Barradas, Ana M. C.; de Ruiter, Ad; Walsh, William R.; van Blitterswijk, Clemens A.; de Bruijn, Joost D.

2010-01-01

Biomaterials can be endowed with biologically instructive properties by changing basic parameters such as elasticity and surface texture. However, translation from in vitro proof of concept to clinical application is largely missing. Porous calcium phosphate ceramics are used to treat small bone defects but in general do not induce stem cell differentiation, which is essential for regenerating large bone defects. Here, we prepared calcium phosphate ceramics with varying physicochemical and structural characteristics. Microporosity correlated to their propensity to stimulate osteogenic differentiation of stem cells in vitro and bone induction in vivo. Implantation in a large bone defect in sheep unequivocally demonstrated that osteoinductive ceramics are equally efficient in bone repair as autologous bone grafts. Our results provide proof of concept for the clinical application of “smart” biomaterials. PMID:20643969

Strong emission in Yb3+/Er3+ co-doped phosphate glass ceramics

NASA Astrophysics Data System (ADS)

Liu, Yanling; Song, Feng; Jia, Guozhi; Zhang, Yanbang; Tang, Yi

Yb3+/Er3+ co-doped phosphate glass and glass ceramics were prepared by high-temperature melting method. The X-ray diffraction, transmission electron micrographs, up-conversion and infrared emissions, photothermal conversion properties of the samples have been measured. The results showed the annealing time had a great impact on the microstructure and luminous performance of the phosphate glass. At the beginning of annealing, the metaphosphate crystals were firstly dissolved out. The metaphosphate crystals gradually turned into the orthophosphate with the increasing of annealing time. The emission intensity of the sample was obviously improved after the precursor glass was annealed. The up-conversion and infrared emissions of the sample annealed at 600 °C for 24 h, reached the maximum intensity. Compared with the photothermal properties of glass, the lower photothermal conversion efficiency of the glass ceramics testified the strong emission.

Modeling of multiphase flow with solidification and chemical reaction in materials processing

NASA Astrophysics Data System (ADS)

Wei, Jiuan

Understanding of multiphase flow and related heat transfer and chemical reactions are the keys to increase the productivity and efficiency in industrial processes. The objective of this thesis is to utilize the computational approaches to investigate the multiphase flow and its application in the materials processes, especially in the following two areas: directional solidification, and pyrolysis and synthesis. In this thesis, numerical simulations will be performed for crystal growth of several III-V and II-VI compounds. The effects of Prandtl and Grashof numbers on the axial temperature profile, the solidification interface shape, and melt flow are investigated. For the material with high Prandtl and Grashof numbers, temperature field and growth interface will be significantly influenced by melt flow, resulting in the complicated temperature distribution and curved interface shape, so it will encounter tremendous difficulty using a traditional Bridgman growth system. A new design is proposed to reduce the melt convection. The geometric configuration of top cold and bottom hot in the melt will dramatically reduce the melt convection. The new design has been employed to simulate the melt flow and heat transfer in crystal growth with large Prandtl and Grashof numbers and the design parameters have been adjusted. Over 90% of commercial solar cells are made from silicon and directional solidification system is the one of the most important method to produce multi-crystalline silicon ingots due to its tolerance to feedstock impurities and lower manufacturing cost. A numerical model is developed to simulate the silicon ingot directional solidification process. Temperature distribution and solidification interface location are presented. Heat transfer and solidification analysis are performed to determine the energy efficiency of the silicon production furnace. Possible improvements are identified. The silicon growth process is controlled by adjusting heating power and moving the side insulation layer upward. It is possible to produce high quality crystal with a good combination of heating and cooling. SiC based ceramic materials fabricated by polymer pyrolysis and synthesis becomes a promising candidate for nuclear applications. To obtain high uniformity of microstructure/concentration fuel without crack at high operating temperature, it is important to understand transport phenomena in material processing at different scale levels. In our prior work, a system level model based on reactive porous media theory was developed to account for the pyrolysis process in uranium-ceramic nuclear fabrication In this thesis, a particle level mesoscopic model based on the Smoothed Particle Hydrodynamics (SPH) is developed for modeling the synthesis of filler U3O8 particles and SiC matrix. The system-level model provides the thermal boundary conditions needed in the particle level simulation. The evolution of particle concentration and structure as well as composition of composite produced will be investigated. Since the process temperature and heat flux play the important roles in material quality and uniformity, the effects of heating rate at different directions, filler particle size and distribution on uniformity and microstructure of the final product are investigated. Uncertainty issue is also discussed. For the multiphase flow with directional solidification, a system level based on FVM is established. In this model, melt convection, temperature distribution, phase change and solidification interface can be investigated. For the multiphase flow with chemical reaction, a particle level model based on SPH method is developed to describe the pyrolysis and synthesis process of uranium-ceramic nuclear fuel. Due to its mesh-free nature, SPH can easily handle the problems with multi phases and components, large deformation, chemical reactions and even solidifications. A multi-scale meso-macroscopic approach, which combine a mesoscopic model based on SPH method and macroscopic model based on FVM, FEM and FDM, can be applied to even more complicated system. In the mesoscopic model by SPH method, some fundamental mesoscopic phenomena, such as the microstructure evolution, interface morphology represented by high resolution, particle entrapment in solidification can be studied. In the macroscopic model, the heat transfer, fluid flow, species transport can be modeled, and the simulation results provided the velocity, temperature and species boundary condition necessary for the mesoscopic model. This part falls into the region of future work. (Abstract shortened by UMI.)

Influence of lead on stabilization/solidification by ordinary Portland cement and magnesium phosphate cement.

PubMed

Wang, Yan-Shuai; Dai, Jian-Guo; Wang, Lei; Tsang, Daniel C W; Poon, Chi Sun

2018-01-01

Inorganic binder-based stabilization/solidification (S/S) of Pb-contaminated soil is a commonly used remediation approach. This paper investigates the influences of soluble Pb species on the hydration process of two types of inorganic binders: ordinary Portland cement (OPC) and magnesium potassium phosphate cement (MKPC). The environmental leachability, compressive strength, and setting time of the cement products are assessed as the primary performance indicators. The mechanisms of Pb involved in the hydration process are analyzed through X-ray diffraction (XRD), hydration heat evolution, and thermogravimetric analyses. Results show that the presence of Pb imposes adverse impact on the compressive strength (decreased by 30.4%) and the final setting time (prolonged by 334.7%) of OPC, but it exerts much less influence on those of MKPC. The reduced strength and delayed setting are attributed to the retarded hydration reaction rate of OPC during the induction period. These results suggest that the OPC-based S/S of soluble Pb mainly depends on physical encapsulation by calcium-silicate-hydrate (CSH) gels. In contrast, in case of MKPC-based S/S process, chemical stabilization with residual phosphate (pyromorphite and lead phosphate precipitation) and physical fixation of cementitious struvite-K are the major mechanisms. Therefore, MKPC is a more efficient and chemically stable inorganic binder for the Pb S/S process. Copyright © 2017 Elsevier Ltd. All rights reserved.

Bioactive calcium phosphate–based glasses and ceramics and their biomedical applications: A review

PubMed Central

Islam, Md Towhidul; Felfel, Reda M; Abou Neel, Ensanya A; Grant, David M; Ahmed, Ifty; Hossain, Kazi M Zakir

2017-01-01

An overview of the formation of calcium phosphate under in vitro environment on the surface of a range of bioactive materials (e.g. from silicate, borate, and phosphate glasses, glass-ceramics, bioceramics to metals) based on recent literature is presented in this review. The mechanism of bone-like calcium phosphate (i.e. hydroxyapatite) formation and the test protocols that are either already in use or currently being investigated for the evaluation of the bioactivity of biomaterials are discussed. This review also highlights the effect of chemical composition and surface charge of materials, types of medium (e.g. simulated body fluid, phosphate-buffered saline and cell culture medium) and test parameters on their bioactivity performance. Finally, a brief summary of the biomedical applications of these newly formed calcium phosphate (either in the form of amorphous or apatite) is presented. PMID:28794848

Effect of raw material ratios on the compressive strength of magnesium potassium phosphate chemically bonded ceramics.

PubMed

Wang, Ai-juan; Yuan, Zhi-long; Zhang, Jiao; Liu, Lin-tao; Li, Jun-ming; Liu, Zheng

2013-12-01

The compressive strength of magnesium potassium phosphate chemically bonded ceramics is important in biomedical field. In this work, the compressive strength of magnesium potassium phosphate chemically bonded ceramics was investigated with different liquid-to-solid and MgO-to-KH2PO4 ratios. X-ray diffractometer was applied to characterize its phase composition. The microstructure was imaged using a scanning electron microscope. The results showed that the compressive strength of the chemically bonded ceramics increased with the decrease of liquid-to-solid ratio due to the change of the packing density and the crystallinity of hydrated product. However, with the increase of MgO-to-KH2PO4 weight ratio, its compressive strength increased firstly and then decreased. The low compressive strength in lower MgO-to-KH2PO4 ratio might be explained by the existence of the weak phase KH2PO4. However, the low value of compressive strength with the higher MgO-to-KH2PO4 ratio might be caused by lack of the joined phase in the hydrated product. Besides, it has been found that the microstructures were different in these two cases by the scanning electron microscope. Colloidal structure appeared for the samples with lower liquid-to-solid and higher MgO-to-KH2PO4 ratios possibly because of the existence of amorphous hydrated products. The optimization of both liquid-to-solid and MgO-to-KH2PO4 ratios was important to improve the compressive strength of magnesium potassium phosphate chemically bonded ceramics. © 2013.

Simple additive manufacturing of an osteoconductive ceramic using suspension melt extrusion.

PubMed

Slots, Casper; Jensen, Martin Bonde; Ditzel, Nicholas; Hedegaard, Martin A B; Borg, Søren Wiatr; Albrektsen, Ole; Thygesen, Torben; Kassem, Moustapha; Andersen, Morten Østergaard

2017-02-01

Craniofacial bone trauma is a leading reason for surgery at most hospitals. Large pieces of destroyed or resected bone are often replaced with non-resorbable and stock implants, and these are associated with a variety of problems. This paper explores the use of a novel fatty acid/calcium phosphate suspension melt for simple additive manufacturing of ceramic tricalcium phosphate implants. A wide variety of non-aqueous liquids were tested to determine the formulation of a storable 3D printable tricalcium phosphate suspension ink, and only fatty acid-based inks were found to work. A heated stearic acid-tricalcium phosphate suspension melt was then 3D printed, carbonized and sintered, yielding implants with controllable macroporosities. Their microstructure, compressive strength and chemical purity were analyzed with electron microscopy, mechanical testing and Raman spectroscopy, respectively. Mesenchymal stem cell culture was used to assess their osteoconductivity as defined by collagen deposition, alkaline phosphatase secretion and de-novo mineralization. After a rapid sintering process, the implants retained their pre-sintering shape with open pores. They possessed clinically relevant mechanical strength and were chemically pure. They supported adhesion of mesenchymal stem cells, and these were able to deposit collagen onto the implants, secrete alkaline phosphatase and further mineralize the ceramic. The tricalcium phosphate/fatty acid ink described here and its 3D printing may be sufficiently simple and effective to enable rapid, on-demand and in-hospital fabrication of individualized ceramic implants that allow clinicians to use them for treatment of bone trauma. Copyright © 2016 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Canister, Sealing Method And Composition For Sealing A Borehole

DOEpatents

Brown, Donald W.; Wagh, Arun S.

2005-06-28

Method and composition for sealing a borehole. A chemically bonded phosphate ceramic sealant for sealing, stabilizing, or plugging boreholes is prepared by combining an oxide or hydroxide and a phosphate with water to form slurry. The slurry is introduced into the borehole where the seal, stabilization or plug is desired, and then allowed to set up to form the high strength, minimally porous sealant, which binds strongly to itself and to underground formations, steel and ceramics.

Survey and research on up-conversion emission character and energy transition of Yb3+/Er3+/Tm3+ co-doped phosphate glass and glass ceramic

NASA Astrophysics Data System (ADS)

Yu, Yin; Song, Feng; Ming, Chengguo; Liu, Jiadong; Li, Wei; Liu, Yanling; Zhao, Hongyan

2012-11-01

By conventional high-temperature melting method, Yb3+/Er3+/Tm3+ co-doped phosphate glass was synthesized. After annealing the precursor glass, the phosphate glass ceramic (GC) was obtained. By measuring the X-ray diffraction (XRD) spectrum, it is proved that the LiYbP4O12 and Li6P6O18 nano-crystals have existed in the phosphate GC. The up-conversion (UC) emission intensity of the GC is obvious stronger compared to that of the glass. The reason is that the shorter distance between rare earth ions in the glass ceramic increases the energy transitions from the sensitized ions (Yb3+) to the luminous ions (Er3+ and Tm3+). By studying the dependence of UC emissions on the pump power, the 523 and 546 nm green emissions of Er3+ ions in the glass are two-photon processes. But in the glass ceramic, they are two/three-photon processes. The phenomenon implies that a three-photon process has participated in the population of the two green emissions. Using Dexter theory, we discuss the energy transitions of Er3+ and Tm3+. The results indicate the energy transition of Tm3+ to Er3+ is very strong in the GC, which changes the population mechanism of UC emissions of Er3+.

Polymer-Ceramic Composite Scaffolds: The Effect of Hydroxyapatite and β-tri-Calcium Phosphate

PubMed Central

Caetano, Guilherme; Vyas, Cian; Diver, Carl; Bártolo, Paulo

2018-01-01

The design of bioactive scaffolds with improved mechanical and biological properties is an important topic of research. This paper investigates the use of polymer-ceramic composite scaffolds for bone tissue engineering. Different ceramic materials (hydroxyapatite (HA) and β-tri-calcium phosphate (TCP)) were mixed with poly-ε-caprolactone (PCL). Scaffolds with different material compositions were produced using an extrusion-based additive manufacturing system. The produced scaffolds were physically and chemically assessed, considering mechanical, wettability, scanning electron microscopy and thermal gravimetric tests. Cell viability, attachment and proliferation tests were performed using human adipose derived stem cells (hADSCs). Results show that scaffolds containing HA present better biological properties and TCP scaffolds present improved mechanical properties. It was also possible to observe that the addition of ceramic particles had no effect on the wettability of the scaffolds. PMID:29342890

Self Assembled Structures by Directional Solidification of Eutectics

NASA Technical Reports Server (NTRS)

Dynys, Frederick W.; Sayir, Ali

2004-01-01

Interest in ordered porous structures has grown because of there unique properties such as photonic bandgaps, high backing packing density and high surface to volume ratio. Inspired by nature, biometric strategies using self assembled organic molecules dominate the development of hierarchical inorganic structures. Directional solidification of eutectics (DSE) also exhibit self assembly characteristics to form hierarchical metallic and inorganic structures. Crystallization of diphasic materials by DSE can produce two dimensional ordered structures consisting of rods or lamella. By selective removal of phases, DSE is capable to fabricate ordered pore arrays or ordered pin arrays. Criteria and limitations to fabricate hierarchical structures will be presented. Porous structures in silicon base alloys and ceramic systems will be reported.

Production of porous Calcium Phosphate (CaP) ceramics with aligned pores using ceramic/camphene-based co-extrusion.

PubMed

Choi, Won-Young; Kim, Hyoun-Ee; Moon, Young-Wook; Shin, Kwan-Ha; Koh, Young-Hag

2015-01-01

Calcium phosphate (CaP) ceramics are one of the most valuable biomaterials for uses as the bone scaffold owing to their outstanding biocompatability, bioactivity, and biodegradation nature. In particular, these materials with an open porous structure can stimulate bone ingrowth into their 3-dimensionally interconnected pores. However, the creation of pores in bulk materials would inevitably cause a severe reduction in mechanical properties. Thus, it is a challenge to explore new ways of improving the mechanical properties of porous CaP scaffolds without scarifying their high porosity. Porous CaP ceramic scaffolds with aligned pores were successfully produced using ceramic/camphene-based co-extrusion. This aligned porous structure allowed for the achievement of high compressive strength when tested parallel to the direction of aligned pores. In addition, the overall porosity and mechanical properties of the aligned porous CaP ceramic scaffolds could be tailored simply by adjusting the initial CaP content in the CaP/camphene slurry. The porous CaP scaffolds showed excellent in vitro biocompatibility, suggesting their potential as the bone scaffold. Aligned porous CaP ceramic scaffolds with considerably enhanced mechanical properties and tailorable porosity would find very useful applications as the bone scaffold.

Evaluation of biocompatibility of various ceramic powders with human fibroblasts in vitro.

PubMed

Li, J; Liu, Y; Hermansson, L; Söremark, R

1993-01-01

Cell reaction to powders of ceramics was studied in vitro. Cultured human fibroblasts were exposed to different types of ceramic powders: zirconia (ZP), alumina (A), tricalcium phosphate (TCP) and hydroxyapatite (HA), at various concentrations. The cell viability at the different exposure times was measured by the colony formation (expressed as colony forming efficiency, CFE), neutral red uptake (NR) and colorimetric tetrazolium (MTT) reduction. Alumina and hydroxyapatite showed no cytotoxic effects at studied doses (1-500 mug/ml) while zirconia and tricalcium phosphate inhibited cell viability, with 50% of CFE reduction at the concentration of about 50 mug/ml. In order to study the cytotoxic mechanism of zirconia powder, two further experiments were included, viz. the cellular response to the sintered zirconia ceramic powders (CZP) which were obtained by crushing the sintered ceramic material; and the measurement of the degradation of zirconia ceramic plate in the different solutions, i.e., either in saline or in 0.02 M lactic acid (pH 2.72). Similar cell reactions were obtained for the CZP and ZP by using MTT and NR assays. Slow releases of ions from zirconia ceramic plate, yttrium in both solutions and zirconium and yttrium in lactic acid, were detected.

[Effects of simulated body fluid flowing rate on bone-like apatite formation on porous calcium phosphate ceramics].

PubMed

Duan, You-rong; Liu, Ke-wei; Chen, Ji-yong; Zhang, Xing-dong

2002-06-01

Objective. Bone-like apatite formation on the surface of calcium phosphate ceramics was believed to be the necessary step that new bone grows on the ceramics and to be relative to the osteoinductivity of the material. This study aimed at investigating the influence of the flow rate of simulated body fluid (SBF) (2 ml/min) in skeletal muscle upon the formation of bone-like apatite on porous calcium phosphate ceramics. Method. The dynamic condition was realized by controlling the SBF flowing in/out of the sample chamber of 100 ml. The flow rate of 2 ml/min is close to that in human muscle environment. The pH and inorganic ionic composition of SBF are close to those of human body fluid. Result. Bone-like apatite formation was relatively easier to occur in static SBF than in dynamic SBF. Experiment with flowing SBF (dynamic SBF) is better in mimicking the living body fluid than static SBF. Conclusion. The results from dynamic SBF may more truly show the relation between apatite layer formation and osteoinduction in biomaterials than that from in vitro experiments before.

Vitrified chemically bonded phosphate ceramics for immobilization of radioisotopes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wagh, Arun S.

2016-04-05

A method of immobilizing a radioisotope and vitrified chemically bonded phosphate ceramic (CBPC) articles formed by the method are described. The method comprises combining a radioisotope-containing material, MgO, a source of phosphate, and optionally, a reducing agent, in water at a temperature of less than 100.degree. C. to form a slurry; curing the slurry to form a solid intermediate CBPC article comprising the radioisotope therefrom; comminuting the intermediate CBPC article, mixing the comminuted material with glass frits, and heating the mixture at a temperature in the range of about 900 to about 1500.degree. C. to form a vitrified CBPC articlemore » comprising the radioisotope immobilized therein.« less

Progress on Numerical Modeling of the Dispersion of Ceramic Nanoparticles During Ultrasonic Processing and Solidification of Al-Based Nanocomposites

NASA Astrophysics Data System (ADS)

Zhang, Daojie; Nastac, Laurentiu

2016-12-01

In present study, 6061- and A356-based nano-composites are fabricated by using the ultrasonic stirring technology (UST) in a coreless induction furnace. SiC nanoparticles are used as the reinforcement. Nanoparticles are added into the molten metal and then dispersed by ultrasonic cavitation and acoustic streaming assisted by electromagnetic stirring. The applied UST parameters in the current experiments are used to validate a recently developed magneto-hydro-dynamics (MHD) model, which is capable of modeling the cavitation and nanoparticle dispersion during UST processing. The MHD model accounts for turbulent fluid flow, heat transfer and solidification, and electromagnetic field, as well as the complex interaction between the nanoparticles and both the molten and solidified alloys by using ANSYS Maxwell and ANSYS Fluent. Molecular dynamics (MD) simulations are conducted to analyze the complex interactions between the nanoparticle and the liquid/solid interface. The current modeling results demonstrate that a strong flow can disperse the nanoparticles relatively well during molten metal and solidification processes. MD simulation results prove that ultrafine particles (10 nm) will be engulfed by the solidification front instead of being pushed, which is beneficial for nano-dispersion.

BMP-7 Preserves Surface Integrity of Degradable-ceramic Cranioplasty in a Göttingen Minipig Model

PubMed Central

Schulz, Peter; Klünter, Tim; Deisinger, Ulrike; Diez, Claudius; Waiss, Waltraud; Kirschneck, Christian; Reichert, Torsten E.; Detsch, Rainer

2017-01-01

Background: The aim of the study was to evaluate the integrity of a craniotomy grafted site in a minipig model using different highly porous calcium phosphate ceramic scaffolds either loaded or nonloaded with bone morphogenetic protein-7 (BMP-7). Methods: Four craniotomies with a diameter of 15 mm (critical-size defect) were grafted with different highly porous (92–94 vol%) calcium phosphate ceramics [hydroxyapatite (HA), tricalcium phosphate (TCP), and biphasic calcium phosphate (BCP; a mixture of HA and TCP)] in 10 Göttingen minipigs: (a) group I (n = 5): HA versus BCP; (b) group II (n = 5): TCP versus BCP. One scaffold of each composition was supplied with 250 μg of BMP-7. In vivo computed tomography scan and fluorochrome bone labeling were performed. Specimens were evaluated 14 weeks after surgery by environmental scanning electron microscopy, fluorescence microscopy, and Giemsa staining histology. Results: BMP-7 significantly enhanced bone formation in TCP (P = 0.047). Slightly enhanced bone formation was observed in BCP (P = 0.059) but not in HA implants. BMP-7 enhanced ceramic degradation in TCP (P = 0.05) and BCP (P = 0.05) implants but not in HA implants. Surface integrity of grafted site was observed in all BMP-7-loaded implants after successful creeping substitution by the newly formed bone. In 9 of 10 HA implants without BMP-7, partial collapse of the implant site was observed. All TCP implants without BMP-7 collapsed. Fluorescent labeling showed bone formation at week 1 in BMP-7-stimulated implants. Conclusions: BMP-7 supports bone formation, ceramic degradation, implant integration, and surface integrity of the grafted site. PMID:28458969

Bone Morphogenetic Protein-7 Enhances Degradation of Osteoinductive Bioceramic Implants in an Ectopic Model

PubMed Central

Klünter, Tim; Schulz, Peter; Deisinger, Ulrike; Diez, Claudius; Waiss, Waltraud; Kirschneck, Christian; Reichert, Torsten E.; Detsch, Rainer

2017-01-01

Background: The aim of the present study was to evaluate the degradation pattern of highly porous bioceramics as well as the bone formation in presence of bone morphogenetic protein 7 (BMP-7) in an ectopic site. Methods: Novel calcium phosphate ceramic cylinders sintered at 1,300°C with a total porosity of 92–94 vol%, 45 pores per inch, and sized 15 mm (Ø) × 5 mm were grafted on the musculus latissimus dorsi bilaterally in 10 Göttingen minipigs: group I (n = 5): hydroxyapatite (HA) versus biphasic calcium phosphate (BCP), a mixture of HA and tricalcium phosphate (TCP) in a ratio of 60/40 wt%; group II (n = 5): TCP versus BCP. A test side was supplied in situ with 250 μg BMP-7. Fluorochrome bone labeling and computed tomography were performed in vivo. Specimens were evaluated 14 weeks after surgery by environmental scanning electron microscopy, fluorescence microscopy, tartrate-resistant acid phosphatase, and pentachrome staining. Results: Bone formation was enhanced in the presence of BMP-7 in all ceramics (P = 0.001). Small spots of newly formed bone were observed in all implants in the absence of BMP-7. Degradation of HA and BCP was enhanced in the presence of BMP-7 (P = 0.001). In those ceramics, osteoclasts were observed. TCP ceramics were almost completely degraded independently of the effect of BMP-7 after 14 weeks (P = 0.76), osteoclasts were not observed. Conclusions: BMP-7 enhanced bone formation and degradation of HA and BCP ceramics via osteoclast resorption. TCP degraded via dissolution. All ceramics were osteoinductive. Novel degradable HA and BCP ceramics in the presence of BMP-7 are promising bone substitutes in the growing individual. PMID:28740783

Experimental and in silico investigations of organic phosphates and phosphonates sorption on polymer-ceramic monolithic materials and hydroxyapatite.

PubMed

Pietrzyńska, Monika; Zembrzuska, Joanna; Tomczak, Rafał; Mikołajczyk, Jakub; Rusińska-Roszak, Danuta; Voelkel, Adam; Buchwald, Tomasz; Jampílek, Josef; Lukáč, Miloš; Devínsky, Ferdinand

2016-10-10

A method based on experimental and in silico evaluations for investigating interactions of organic phosphates and phosphonates with hydroxyapatite was developed. This quick and easy method is used for determination of differences among organophosphorus compounds of various structures in their mineral binding affinities. Empirical sorption evaluation was carried out using liquid chromatography with tandem mass spectrometry or UV-VIS spectroscopy. Raman spectroscopy was used to confirm sorption of organic phosphates and phosphonates on hydroxyapatite. Polymer-ceramic monolithic material and bulk hydroxyapatite were applied as sorbent materials. Furthermore, a Polymer-ceramic Monolithic In-Needle Extraction device was used to investigate both sorption and desorption steps. Binding energies were computed from the fully optimised structures utilising Density Functional Theory (DFT) at B3LYP/6-31+G(d,p) level. Potential pharmacologic and toxic effects of the tested compounds were estimated by the Prediction of the Activity Spectra of Substances using GeneXplain software. Copyright © 2016 Elsevier B.V. All rights reserved.

Sodium aluminum-iron phosphate glass-ceramics for immobilization of lanthanide oxide wastes from pyrochemical reprocessing of spent nuclear fuel

NASA Astrophysics Data System (ADS)

Stefanovsky, S. V.; Stefanovsky, O. I.; Kadyko, M. I.; Nikonov, B. S.

2018-03-01

Sodium aluminum (iron) phosphate glass ceramics containing of up to 20 wt.% rare earth (RE) oxides simulating pyroprocessing waste were produced by melting at 1250 °C followed by either quenching or slow cooling to room temperature. The iron-free glass-ceramics were composed of major glass and minor phosphotridymite and monazite. The iron-bearing glass-ceramics were composed of major glass and minor monazite and Na-Al-Fe orthophosphate at low waste loadings (5-10 wt.%) and major orthophosphate and minor monazite as well as interstitial glass at high waste loadings (15-20 wt.%). Slowly cooled samples contained higher amount of crystalline phases than quenched ones. Monazite is major phase for REs. Leach rates from the materials of major elements (Na, Al, Fe, P) are 10-5-10-7 g cm-2 d-1, RE elements - lower than 10-5 g cm-2 d-1.

Silicon-based Porous Ceramics via Freeze Casting of Preceramic Polymers

NASA Astrophysics Data System (ADS)

Naviroj, Maninpat

Freeze casting is a technique for processing porous materials that has drawn significant attention for its effectiveness in producing a variety of tailorable pore structures for ceramics, metals, and polymers. With freeze casting, pores are generated based on a solidification process where ice crystals act as a sacrificial template which can eventually be sublimated to create pores. While the majority of freeze-casting studies have been performed using conventional ceramic suspensions, this work explores an alternative processing route by freeze casting with preceramic polymer solutions. Significant differences exist between freeze casting of a particulate suspension and a polymeric solution. These changes affect the processing method, solidification behavior, and pore structure, thereby introducing new challenges and possibilities for the freeze-casting technique. The first part of this study explored the processing requirements involved with freeze casting of preceramic polymers, along with methods to control the resulting pore structure. Solvent choice, freezing front velocity, and polymer concentration were used as processing variables to manipulate the pore structures. A total of seven organic solvents were freeze cast with a polymethylsiloxane preceramic polymer to produce ceramics with isotropic, dendritic, prismatic, and lamellar pore morphologies. Changes in freezing front velocity and polymer concentration were shown to influence pore size, shape, and connectivity. Differences between suspension- and solution-based samples freeze cast under equivalent conditions were also investigated. Certain solidification microstructures were strongly affected by the presence of suspended particles, creating differences between pore structures generated from the same solvents. Additionally, processing of solution-based samples were found to be the more facile technique. Compressive strength and water permeability of dendritic and lamellar structures were analyzed to determine functional differences between the pore structures. Results show that dendritic structures were up to 30 times stronger, while lamellar structures provided higher permeability constants. A change in freezing front velocity was shown to significantly affect permeability but not compressive strength. Finally, improved pore alignment along the freezing direction was achieved by controlling the nucleation and growth of solvent crystals through the use of a grain-selection template. Dendritic samples freeze cast with a template showed substantial increase in pore alignment, as determined by image analysis and permeability tests, with the permeability constant increasing by up to 6-fold when compared to a control sample.

Resorption kinetics of four hydroxyapatite-based ceramics by particle induced X-ray emission and neutron activation analysis

NASA Astrophysics Data System (ADS)

Jallot, E.; Irigaray, J. L.; Oudadesse, H.; Brun, V.; Weber, G.; Frayssinet, P.

1999-05-01

From the viewpoint of hard tissue response to implant materials, calcium phosphates are probably the most compatible materials presently known. During the last few years, much attention has been paid to hydroxyapatite and β-tricalcium phosphate as potential biomaterials for bone substitute. A good implantation of biomaterials in the skeleton is to reach full integration of non-living implant with living bone. The aim of this study is to compare the resorption kinetics of four kinds of calcium phosphate ceramics: hydroxyapatite (Ca{10}(PO4)6(OH)2), hydroxyapatite doped with manganese or zinc and a composite material of 75% hydroxyapatite and 25% β-tricalcium phosphate (Ca3(PO4)2). Cylinders (5 6 mm in diameter) of these ceramics were packed into holes made in the femur diaphysis of mature ovine. At 2, 4, 8, 12, 16, 20, 28, 36 and 48 weeks after the operation, bone/implant interface was embedded in polymethylmethacrylate. We used the PIXE method (particle induced X-ray emission) to measure the distribution of mineral elements (Ca, P, Sr, Zn, Mn and Fe) at the bone/implant interface. At 4, 8, 16, 28 and 48 weeks after implantation we studied a biopsy of the ceramics by neutron activation method. Then, we have a global measurement of mineral elements in the biomaterial. The results showed that the resorption kinetics of hydroxyapatite doped with zinc was faster than that of the three other bioceramics.

Cr-Free Metallic-Ceramic Coatings

DTIC Science & Technology

2014-11-01

Comparable to Aluminum-Chromate/ Phosphate Humidity Resistance Galvanic Corrosion Resistance Nov. 2014 ASETSDefense 2014, Fort Myer, VA...Aluminum-Silicate Comparable to Aluminum-Chromate/ Phosphate  Humidity, Galvanic Corrosion , Heat/Salt Resistance  Adhesion & Compatibility...WP-TR-2007-4069, Sept. 2006 Sealed Aluminum-Silicate Not Comparable to Sealed Aluminum-Chromate/ Phosphate in PEWG Evaluation  Corrosion

3D microenvironment as essential element for osteoinduction by biomaterials.

PubMed

Habibovic, Pamela; Yuan, Huipin; van der Valk, Chantal M; Meijer, Gert; van Blitterswijk, Clemens A; de Groot, Klaas

2005-06-01

In order to unravel the mechanism of osteoinduction by biomaterials, in this study we investigated the influence of the specific surface area on osteoinductive properties of two types of calcium phosphate ceramics. Different surface areas of the ceramics were obtained by varying their sintering temperatures. Hydroxyapatite (HA) ceramic was sintered at 1150 and 1250 degrees C. Biphasic calcium phosphate (BCP) ceramic, consisting of HA and beta-tricalcium phosphate (beta-TCP), was sintered at 1100, 1150 and 1200 degrees C. Changes in sintering temperature did not influence the chemistry of the ceramics; HA remained pure after sintering at different temperatures and the weight ratio of HA and beta-TCP in the BCP was independent of the temperature as well. Similarly, macroporosity of the ceramics was unaffected by the changes of the sintering temperature. However, microporosity (pore diameter <10 microm) significantly decreased with increasing sintering temperature. In addition to the decrease of the microporosity, the crystal size increased with increasing sintering temperature. These two effects resulted in a significant decrease of the specific surface area of the ceramics with increasing sintering temperatures. Samples of HA1150, HA1250, BCP1100, BCP1150 and BCP1200 were implanted in the back muscles of Dutch milk goats and harvested at 6 and 12 weeks post implantation. After explantation, histomorphometrical analysis was performed on all implants. All implanted materials except HA1250 induced bone. However, large variations in the amounts of induced bone were observed between different materials and between individual animals. Histomorphometrical results showed that the presence of micropores within macropore walls is necessary to make a material osteoinductive. We postulate that introduction of microporosity within macropores, and consequent increase of the specific surface area, affects the interface dynamics of the ceramic in such a way that relevant cells are triggered to differentiate into the osteogenic lineage.

Preparation and characterization of calcium phosphate ceramics and composites as bone substitutes

NASA Astrophysics Data System (ADS)

Zhang, Xing

Marine CaCO3 skeletons have tailored architectures created by nature, which give them structural support and other functions. For example, seashells have dense lamellar structures, while coral, cuttlebone and sea urchin spines have interconnected porous structures. In our experiments, seashells, coral and cuttlebone were hydrothermally converted to hydroxyapatite (HAP), and sea urchin spines were converted to Mg-substituted tricalcium phosphate (beta-TCMP), while maintaining their original structures. Partially converted shell samples have mechanical strength, which is close to that of compact human bone. After implantation of converted shell and spine samples in rat femoral defects for 6 weeks, there was newly formed bone growth up to and around the implants. Some new bone was found to migrate through the pores of converted spine samples and grow inward. These results show good bioactivity and osteoconductivity of the implants, indicating the converted shell and spine samples can be used as bone defect fillers. Calcium phosphate powders were prepared through different synthesis methods. Micro-size HAP rods were synthesized by hydrothermal method through a nucleation-growth mechanism. On the other hand, HAP particles, which have good crystallinity, were prepared by wet precipitation with further hydrothermal treatment. beta-TCP or beta-TCMP powders were prepared by a two-step process: wet precipitation of apatitic tricalcium phosphate ('precursor') and calcination of the precursor at 800°C for 3 hours. beta-TCMP or beta-TCP powders were also prepared by solid-state reactions from CaHPO4 and CaCO 3 with/without MgO. Biphasic calcium phosphate, which is mixture of HAP and beta-TCP, can be prepared though mechanical mixing of HAP and beta-TCP powders synthesized as above. Dense beta-TCP and beta-TCMP ceramics can be produced by pressing green bodies at 100MPa and further sintering above 1100°C for 2 hours. beta-TCMP ceramics ˜99.4% relative dense were prepared by this method. Dense beta-TCP ceramics have average strength up to 540MPa. Macroporous beta-TCMP ceramics were produced with sucrose as the porogen following a two-step pressing method. Porous beta-TCMP ceramics were also prepared by replication of polyurethane sponge. beta-TCMP ceramics with porous structures in the center surrounded by dense structures were created. The outside dense structures give the scaffold mechanical strength, while the central porous structures enable cells migration and vascular infiltration, and finally in-growth of new bone into the scaffold.

Comparison of osteoblast-like cell responses to calcium silicate and tricalcium phosphate ceramics in vitro.

PubMed

Ni, Siyu; Chang, Jiang; Chou, Lee; Zhai, Wanyin

2007-01-01

Calcium silicate ceramics have been proposed as new bone repair biomaterials, since they have proved to be bioactive, degradable, and biocompatible. Beta-tricalcium phosphate ceramic is a well-known degradable material for bone repair. This study compared the effects of CaSiO3 (alpha-, and beta-CaSiO3) and beta-Ca3(PO4)2 (beta-TCP) ceramics on the early stages of rat osteoblast-like cell attachment, proliferation, and differentiation. Osteoblast-like cells were cultured directly on CaSiO3 (alpha-, and beta-CaSiO3) and beta-TCP ceramics. Attachment of a greater number of cells was observed on CaSiO3 (alpha-, and beta-CaSiO3) ceramics compared with beta-TCP ceramics after incubation for 6 h. SEM observations showed an intimate contact between cells and the substrates, significant cells adhesion, and that the cells spread and grew on the surfaces of all the materials. In addition, the proliferation rate and alkaline phosphatase (ALP) activity of the cells on the CaSiO3 (alpha-, and beta-CaSiO3) ceramics were improved when compared with the beta-TCP ceramics. In the presence of CaSiO3, elevated levels of calcium and silicon in the culture medium were observed throughout the 7-day culture period. In conclusion, the results of the present study revealed that CaSiO3 ceramics showed greater ability to support cell attachment, proliferation, and differentiation than beta-TCP ceramic. 2006 Wiley Periodicals, Inc.

Porous biphasic calcium phosphate ceramics coated with nano-hydroxyapatite and seeded with mesenchymal stem cells for reconstruction of radius segmental defects in rabbits.

PubMed

Hu, Jianzhong; Yang, Zhiming; Zhou, Yongchun; Liu, Yong; Li, Kaiyang; Lu, Hongbin

2015-11-01

The osteoconduction of porous biphasic calcium phosphate (BCP) ceramics has been widely reported. In a previous study, we demonstrated that applying a nano-hydroxyapatite (nHA) coating enhances the osteoinductive potential of BCP ceramics, making these scaffolds more suitable for bone tissue engineering applications. The aim of the present study was to determine the effects of reconstructing radius defects in rabbits using nHA-coated BCP ceramics seeded with mesenchymal stem cells (MSCs) and to compare the bone regeneration induced by different scaffolds. Radius defects were created in 20 New Zealand rabbits, which were divided into four groups by treatment: porous BCP ceramics (Group A), nHA-coated porous BCP ceramics (Group B), porous BCP ceramics seeded with rabbit MSCs (Group C), and nHA-coated porous BCP ceramics seeded with rabbit MSCs (Group D). After in vitro incubation, the cell/scaffold complexes were implanted into the defects. Twelve weeks after implantation, the specimens were examined macroscopically and histologically. Both the nHA coating and seeding with MSCs enhanced the formation of new bone tissue in the BCP ceramics, though the osteoinductive potential of the scaffolds with MSCs was greater than that of the nHA-coated scaffolds. Notably, the combination of nHA coating and MSCs significantly improved the bone regeneration capability of the BCP ceramics. Thus, MSCs seeded into porous BCP ceramics coated with nHA may be an effective bone substitute to reconstruct bone defects in the clinic.

Alkali corrosion resistant coatings and ceramic foams having superfine open cell structure and method of processing

DOEpatents

Brown, Jr., Jesse J.; Hirschfeld, Deidre A.; Li, Tingkai

1993-12-07

Alkali corrosion resistant coatings and ceramic foams having superfine open cell structure are created using sol-gel processes. The processes have particular application in creating calcium magnesium zirconium phosphate, CMZP, coatings and foams.

The material and biological characteristics of osteoinductive calcium phosphate ceramics

PubMed Central

Tang, Zhurong; Li, Xiangfeng; Tan, Yanfei

2018-01-01

Abstract The discovery of osteoinductivity of calcium phosphate (Ca-P) ceramics has set an enduring paradigm of conferring biological regenerative activity to materials with carefully designed structural characteristics. The unique phase composition and porous structural features of osteoinductive Ca-P ceramics allow it to interact with signaling molecules and extracellular matrices in the host system, creating a local environment conducive to new bone formation. Mounting evidence now indicate that the osteoinductive activity of Ca-P ceramics is linked to their physicochemical and three-dimensional structural properties. Inspired by this conceptual breakthrough, many laboratories have shown that other materials can be also enticed to join the rank of tissue-inducing biomaterials, and besides the bones, other tissues such as cartilage, nerves and blood vessels were also regenerated with the assistance of biomaterials. Here, we give a brief historical recount about the discovery of the osteoinductivity of Ca-P ceramics, summarize the underlying material factors and biological characteristics, and discuss the mechanism of osteoinduction concerning protein adsorption, and the interaction with different types of cells, and the involvement of the vascular and immune systems. PMID:29423267

Effect of Partial Crystallization on the Structural and Luminescence Properties of Er3+-Doped Phosphate Glasses

PubMed Central

Lopez-Iscoa, Pablo; Salminen, Turkka; Hakkarainen, Teemu; Petit, Laeticia; Janner, Davide; Boetti, Nadia G.; Lastusaari, Mika; Pugliese, Diego; Paturi, Petriina; Milanese, Daniel

2017-01-01

Er-doped phosphate glass ceramics were fabricated by melt-quenching technique followed by a heat treatment. The effect of the crystallization on the structural and luminescence properties of phosphate glasses containing Al2O3, TiO2, and ZnO was investigated. The morphological and structural properties of the glass ceramics were characterized by Field Emission-Scanning Electron Microscopy (FE-SEM), X-ray Diffraction (XRD), and micro-Raman spectroscopy. Additionally, the luminescence spectra and the lifetime values were measured in order to study the influence of the crystallization on the spectroscopic properties of the glasses. The volume ratio between the crystal and the glassy phases increased along with the duration of the heat treatment. The crystallization of the glass ceramics was confirmed by the presence of sharp peaks in the XRD patterns and different crystal phases were identified depending on the glass composition. Sr(PO3)2 crystals were found to precipitate in all the investigated glasses. As evidenced by the spectroscopic properties, the site of the Er3+ ions was not strongly affected by the heat treatment except for the fully crystallized glass ceramic which does not contain Al2O3, TiO2, and ZnO. An increase of the lifetime was also observed after the heat treatment of this glass. Therefore, we suspect that the Er3+ ions are incorporated in the precipitated crystals only in this glass ceramic. PMID:28772833

Short-term effects of mineral particle sizes on cellular degradation activity after implantation of injectable calcium phosphate biomaterials and the consequences for bone substitution.

PubMed

Gauthier, O; Bouler, J M; Weiss, P; Bosco, J; Aguado, E; Daculsi, G

1999-08-01

This in vivo study investigated the influence of two calcium phosphate particle sizes (40-80 microm and 200-500 microm) on the cellular degradation activity associated with the bone substitution process of two injectable bone substitutes (IBS). The tested biomaterials were obtained by associating a biphasic calcium phosphate (BCP) ceramic mineral phase and a 3% aqueous solution of a cellulosic polymer (hydroxypropylmethylcellulose). Both were injected into osseous defects at the distal end of rabbit femurs for 2- and 3-week periods. Quantitative results for tartrate-resistant acid phosphatase (TRAP) cellular activity, new bone formation, and ceramic resorption were studied for statistical purposes. Positive TRAP-stained degradation cells were significantly more numerous for IBS 40-80 than IBS 200-500, regardless of implantation time. BCP degradation was quite marked during the first 2 weeks for IBS 40-80, and bone colonization occurred more extensively for IBS 40-80 than for IBS 200-500. The resorption-bone substitution process occurred earlier and faster for IBS 40-80 than IBS 200-500. Both tested IBS displayed similar biological efficiency, with conserved in vivo bioactivity and bone-filling ability. Differences in calcium phosphate particle sizes influenced cellular degradation activity and ceramic resorption but were compatible with efficient bone substitution.

Wettability and surface free energy of polarised ceramic biomaterials.

PubMed

Nakamura, Miho; Hori, Naoko; Namba, Saki; Toyama, Takeshi; Nishimiya, Nobuyuki; Yamashita, Kimihiro

2015-01-13

The surface modification of ceramic biomaterials used for medical devices is expected to improve osteoconductivity through control of the interfaces between the materials and living tissues. Polarisation treatment induced surface charges on hydroxyapatite, β-tricalcium phosphate, carbonate-substituted hydroxyapatite and yttria-stabilized zirconia regardless of the differences in the carrier ions participating in the polarisation. Characterization of the surfaces revealed that the wettability of the polarised ceramic biomaterials was improved through the increase in the surface free energies compared with conventional ceramic surfaces.

Resorption Rate Tunable Bioceramic: Si, Zn-Modified Tricalcium Phosphate

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wei, Xiang

2006-01-01

This dissertation is organized in an alternate format. Several manuscripts which have already been published or are to be submitted for publication have been included as separate chapters. Chapter 1 is a general introduction which describes the dissertation organization and introduces the human bone and ceramic materials as bone substitute. Chapter 2 is the background and literature review on dissolution behavior of calcium phosphate, and discussion of motivation for this research. Chapter 3 is a manuscript entitled ''Si,Zn-modified tricalcium phosphate: a phase composition and crystal structure study'', which was published in ''Key Engineering Materials'' [1]. Chapter 4 gives more crystalmore » structure details by neutron powder diffraction, which identifies the position for Si and Zn substitution and explains the stabilization mechanism of the structure. A manuscript entitled ''Crystal structure analysis of Si, Zn-modified Tricalcium phosphate by Neutron Powder Diffraction'' will be submitted to Biomaterials [2]. Chapter 5 is a manuscript, entitled ''Dissolution behavior and cytotoxicity test of Si, Zn-modified tricalcium phosphate'', which is to be submitted to Biomaterials [3]. This paper discusses the additives effect on the dissolution behavior of TCP, and cytotoxicity test result is also included. Chapter 6 is the study of hydrolysis process of {alpha}-tricalcium phosphate in the simulated body fluid, and the phase development during drying process is discussed. A manuscript entitled ''Hydrolysis of {alpha}-tricalcium phosphate in simulated body fluid and phase transformation during drying process'' is to be submitted to Biomaterials [4]. Ozan Ugurlu is included as co-authors in these two papers due to his TEM contributions. Appendix A is the general introduction of the materials synthesis, crystal structure and preliminary dissolution result. A manuscript entitled ''Resorption rate tunable bioceramic: Si and Zn-modified tricalcium phosphate'' was published in Ceramic Engineering and Science Proceedings (the 29th International Conference on Advanced Ceramics and Composites - Advances in Bioceramics and Biocomposites) [5].« less

Preparation for microgravity - The role of the Microgravity Material Science Laboratory

NASA Technical Reports Server (NTRS)

Johnston, J. Christopher; Rosenthal, Bruce N.; Meyer, Maryjo B.; Glasgow, Thomas K.

1988-01-01

Experiments at the NASA Lewis Research Center's Microgravity Material Science Laboratory using physical and mathematical models to delineate the effects of gravity on processes of scientific and commercial interest are discussed. Where possible, transparent model systems are used to visually track convection, settling, crystal growth, phase separation, agglomeration, vapor transport, diffusive flow, and polymer reactions. Materials studied include metals, alloys, salts, glasses, ceramics, and polymers. Specific technologies discussed include the General Purpose furnace used in the study of metals and crystal growth, the isothermal dendrite growth apparatus, the electromagnetic levitator/instrumented drop tube, the high temperature directional solidification furnace, the ceramics and polymer laboratories and the center's computing facilities.

Chemically bonded phosphate ceramics of trivalent oxides of iron and manganese

DOEpatents

Wagh, Arun S.; Jeong, Seung-Young

2002-01-01

A new method for combining elemental iron and other metals to form an inexpensive ceramic to stabilize arsenic, alkaline red mud wastes, swarfs, and other iron or metal-based additives, to create products and waste forms which can be poured or dye cast.

Producing Production Level Tooling in Prototype Timing

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mc Hugh, Kevin Matthew; Knirsch, J.

A new rapid solidification process machine will be able to produce eight-inch diameter by six-inch thick finished cavities at the rate of one per hour - a rate that will change the tooling industry dramatically. Global Metal Technologies, Inc. (GMTI) (Solon, OH) has signed an exclusive license with Idaho National Engineered and Environmental Laboratories (INEEL) (Idaho Falls, ID) for the development and commercialization of the rapid solidification process (RSP tooling). The first production machine is scheduled for delivery in July 2001. The RSP tooling process is a method of producing production level tooling in prototype timing. The process' inventor, Kevinmore » McHugh, describes it as a rapid solidification method, which differentiates it from the standard spray forming methods. RSP itself is relatively straightforward. Molten metal is sprayed against the ceramic pattern, replicating the pattern's contours, surface texture and details. After spraying, the molten tool steel is cooled at room temperature and separated from the pattern. The irregular periphery of the freshly sprayed insert is squared off, either by machining or, in the case of harder tool steels, by wire EDM. XX« less

Effect of surface condition of dental zirconia ceramic (Denzir) on bonding.

PubMed

Uo, Motohiro; Sjögren, Göran; Sundh, Anders; Goto, Mitsunari; Watari, Fumio; Bergman, Maud

2006-09-01

Yttria partially stabilized zirconia (YPSZ) ceramics are suitable for dental and medical use because of their high fracture toughness and chemical durability. The purpose of this study was to examine the bonding behavior of a dental YPSZ ceramic, Denzir. After being subjected to various surface treatments, Denzir specimens were bonded to each other using an adhesive resin composite, glass ionomer, or zinc phosphate cement. Bonding strength was then determined by the shearing test. No significant differences (p>0.05) were observed between SiC- and Al2O3-blasted specimens. In all surface treatments, the shear bond strength significantly (p<0.05) increased in the order of adhesive resin composite cement > glass ionomer cement > zinc phosphate cement. Moreover, silanization with methacryloxy propyl trimethoxysilane slightly increased the bonding strength of the adhesive resin composite cement.

Effect of Mg and Si co-substitution on microstructure and strength of tricalcium phosphate ceramics.

PubMed

García-Páez, Ismael H; Carrodeguas, Raúl García; De Aza, Antonio H; Baudín, Carmen; Pena, Pilar

2014-02-01

Magnesium and silicon co-doped tricalcium phosphate (TCP) ceramics with compositions corresponding to 0, 5 and 10wt% CaMg(SiO3)2 in the system Ca3(PO4)2-CaMg(SiO3)2 were obtained by conventional sintering of compacted mixtures of Ca3(PO4)2, MgO, SiO2 and CaCO3 powders at temperatures between 1100 and 1450°C. Microstructural analyses were performed by X-ray diffraction and field emission scanning electron microscopy with energy dispersive spectroscopy. Major phases in the obtained ceramics were β- or α+β-tricalcium phosphate containing Mg and Si in solid solution. Certain amounts of liquid were formed during sintering depending on composition and temperature. There were found significant differences in distributions of strength determined by the diametral compression of disc tests (DCDT). Failure strengths were controlled by microstructural defects associated with phase development. Mg and Si additions were found to be effective to improve densification and associated strength of TCP bioceramics due to the enhancement of sintering by the low viscosity liquids formed. The highest density and strength were obtained for the TCP ceramic containing 5wt% CaMg(SiO3)2 sintered at 1300°C. Cracking and porosity increased at higher temperatures due to grain growth and swelling. © 2013 Published by Elsevier Ltd.

Glass formation and crystallization in the alumina-silica-lanthanum phosphate system for ceramics composites

NASA Astrophysics Data System (ADS)

Guo, Shuling

The formation, structure, and dynamics of glasses in the alumina-silica-lanthanum phosphate system and their crystallization were investigated as a function of composition. These are of interest because of their potential as precursors for synthesizing ceramic-matrix-composites via co-crystallization of lanthanum monazite and either mullite or alumina into finely mixed microstructures. The glasses were characterized by X-Ray Diffraction (XRD), Raman spectroscopy, Differential Scanning Calorimetry (DSC), Nuclear Magnetic Resonance (NMR), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), and Electron Energy Loss Spectrometry (EELS). Glass formation from rapidly quenched liquids was easiest and most consistent for compositions containing silica, such as for mullitemonazite compositions, and more difficult for alumina-monazite compositions. For mullite-monazite glasses, the glass transition temperatures increased linearly from 845°C to 906°C with increasing mullite content. An analysis of the glass structure indicated a network consisting of corner-linked aluminate, silicate and phosphate tetrahedra where aluminum played a central role of separating silicon and phosphorous. It was hypothesized that the glass network consisted of domains of aluminum silicate network edged by phosphate tetrahedra. A maximum in the crystallization temperature was attributed to the complexity of the glass network. At relatively mullite-rich compositions, simultaneous and cooperative crystallization of lanthanum phosphate and mullite correlated with the highest crystallization temperatures, and the lowest activation energies of crystallization. This was preceded by amorphous phase segregation in the glass at lower temperatures. An intermediate phase of lanthanum phosphate was discovered with an orthorhombic unit cell. For compositions of high phosphate contents, lanthanum phosphate precipitated first at about 900°C leaving an essentially pure mullite glass. Mullite crystallized at about 1000°C, matching the conditions for crystallizing pure mullite glass. The phosphate phase transformed to monazite at even higher temperatures. No amorphous phase segregation was observed in these cases. Microstructures were correlated with nucleation and growth conditions such that the continuous and isolated phases could be manipulated. Optimum nucleation temperatures were close to the glass transition temperature. Conditions were identified for forming a continuous boundary phase of monazite that isolated mullite grains, which is desired for fabricating ceramic-matrix-composites.

Role of biphasic calcium phosphate ceramic-mediated secretion of signaling molecules by macrophages in migration and osteoblastic differentiation of MSCs.

PubMed

Wang, Jing; Liu, Dan; Guo, Bo; Yang, Xiao; Chen, Xuening; Zhu, Xiangdong; Fan, Yujiang; Zhang, Xingdong

2017-03-15

The inflammatory reaction initiates fracture healing and could play a role in the osteoinductive effect of calcium phosphate (CaP) ceramics, which has been widely confirmed; however, the underlying mechanism has not been fully elucidated. In this study, various signaling molecules from macrophages under the stimulation of osteoinductive biphasic calcium phosphate (BCP) ceramic and its degradation products were examined and evaluated for their influence on the migration and osteoblastic differentiation of mesenchymal stem cells (MSCs). The results of cellular experiments confirmed that the gene expression of most inflammatory factors (IL-1, IL-6 and MCP-1) and growth factors (VEGF, PDGF and EGF) by macrophages were up-regulated to varying degrees by BCP ceramic and its degradation products. Cell migration tests demonstrated that the conditioned media (CMs), which contained abundant signaling molecules secreted by macrophages cultured on BCP ceramic and its degradation products, promoted the migration of MSCs. qRT-PCR analysis indicated that CMs promoted the gene expression of osteogenic markers (ALP, COL-I, OSX, BSP and OPN) in MSCs. ALP activity and mineralization staining further confirmed that CMs promoted the osteoblastic differentiation of MSCs. The present study confirmed the correlation between the inflammatory reaction and osteoinductive capacity of BCP ceramic. The ceramic itself and its degradation products can induce macrophages to express and secrete various signaling molecules, which then recruit and promote the MSCs to differentiate into osteoblasts. Compared with BCP conditioned media, degradation particles played a more substantial role in this process. Thus, inflammation initiated by BCP ceramic and its degradation products could be necessary for osteoinduction by the ceramic. It is known that the inflammatory reaction initiates fracture healing. The aim of this study was to examine whether osteoinductive BCP ceramics could cause macrophages to change their secretion patterns and whether the secreted cytokines could affect migration and osteoblastic differentiation of MSCs. Moreover, the duration of inflammation could be influenced by the local ionic environment and the degradation products of the implant. Our experimental results revealed the correlation between the inflammatory reaction and osteoinductive capacity of BCP ceramic. The ceramic itself and its degradation products can induce macrophages to express and secrete various signaling molecules, which then recruit and promote the MSCs to differentiate into osteoblasts. Compared with ionic microenvironment, degradation particles played a more substantial role in this process. Therefore, the appropriate inflammation initiated by BCP ceramic and its degradation products could be essential for osteoinduction by the ceramic. We believe that the present study improves the understanding of the effect of biomaterial-mediated inflammation on MSC migration and differentiation and established a preliminary correlation between the immune system and osteoinduction by biomaterials. Copyright © 2017 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Tight ceramic UF membrane as RO pre-treatment: the role of electrostatic interactions on phosphate rejection.

PubMed

Shang, Ran; Verliefde, Arne R D; Hu, Jingyi; Zeng, Zheyi; Lu, Jie; Kemperman, Antoine J B; Deng, Huiping; Nijmeijer, Kitty; Heijman, Sebastiaan G J; Rietveld, Luuk C

2014-01-01

Phosphate limitation has been reported as an effective approach to inhibit biofouling in reverse osmosis (RO) systems for water purification. The rejection of dissolved phosphate by negatively charged TiO2 tight ultrafiltration (UF) membranes (1 kDa and 3 kDa) was observed. These membranes can potentially be adopted as an effective process for RO pre-treatment in order to constrain biofouling by phosphate limitation. This paper focuses on electrostatic interactions during tight UF filtration. Despite the larger pore size, the 3 kDa ceramic membrane exhibited greater phosphate rejection than the 1 kDa membrane, because the 3 kDa membrane has a greater negative surface charge and thus greater electrostatic repulsion against phosphate. The increase of pH from 6 to 8.5 led to a substantial increase in phosphate rejection by both membranes due to increased electrostatic repulsion. At pH 8.5, the maximum phosphate rejections achieved by the 1 kDa and 3 kDa membrane were 75% and 86%, respectively. A Debye ratio (ratio of the Debye length to the pore radius) is introduced in order to evaluate double layer overlapping in tight UF membranes. Threshold Debye ratios were determined as 2 and 1 for the 1 kDa and 3 kDa membranes, respectively. A Debye ratio below the threshold Debye ratio leads to dramatically decreased phosphate rejection by tight UF membranes. The phosphate rejection by the tight UF, in combination with chemical phosphate removal by coagulation, might accomplish phosphate-limited conditions for biological growth and thus prevent biofouling in the RO systems. Copyright © 2013 Elsevier Ltd. All rights reserved.

Development and in vitro examination of materials for osseointegration

NASA Astrophysics Data System (ADS)

Jalota, Sahil

Bone is a connective tissue with nanosized particles of carbonated apatitic calcium phosphate dispersed in a hydrated collagen matrix. With the ageing of the baby boomer population, an increasing number of people sustain bone fractures and defects. Hence, efforts are underway to develop materials to hasten the healing and repairing of such defects. These materials are termed as artificial bone substitutes. This study represents innovative techniques for development of bone implant materials and improving the existing substitute materials. Emphasis was on three different kinds of materials: Metals (titanium and alloys), Ceramics (calcium phosphates), and Polymers (collagen). The bioactivity of titanium and alloys, resorptivity of calcium phosphates and biocompatibility of collagen were the major issues with these materials. These issues are appropriately addressed in this dissertation. For titanium and alloys, biomimetic coating methodology was developed for uniformly and evenly coating 3-D titanium structures. Cracks were observed in these coatings and a protocol was developed to form crack-free biomimetic coatings. In calcium phosphates, increasing the resorption rate of HA (hydroxyapatite) and decreasing the resorption rate of beta-TCP (beta-tricalcium phosphate) were studied. HA-based ceramics were synthesized with Na+ and CO32- ions dopings, and development of biphasic mixtures of HA-beta-TCP and HA-Rhenanite was performed. Similarly, beta-TCP ceramics were synthesized with Zn 2+ ion doping and development of beta-TCP-HA biphasic mixtures was performed. In case of collagen, a biomimetic coating process was developed that decreased the time to coat the collagen substrates and also increased biocompatibility, as determined by the response of mouse osteoblasts.

A safer disposal of hazardous phosphate coating sludge by formation of an amorphous calcium phosphate matrix.

PubMed

Navarro-Blasco, I; Duran, A; Pérez-Nicolás, M; Fernández, J M; Sirera, R; Alvarez, J I

2015-08-15

Phosphate coating hazardous wastes originated from the automotive industry were efficiently encapsulated by an acid-base reaction between phosphates present in the sludge and calcium aluminate cement, yielding very inert and stable monolithic blocks of amorphous calcium phosphate (ACP). Two different compositions of industrial sludge were characterized and loaded in ratios ranging from 10 to 50 wt.%. Setting times and compressive strengths were recorded to establish the feasibility of this method to achieve a good handling and a safe landfilling of these samples. Short solidification periods were found and leaching tests showed an excellent retention for toxic metals (Zn, Ni, Cu, Cr and Mn) and for organic matter. Retentions over 99.9% for Zn and Mn were observed even for loadings as high as 50 wt.% of the wastes. The formation of ACP phase of low porosity and high stability accounted for the effective immobilization of the hazardous components of the wastes. Copyright © 2015 Elsevier Ltd. All rights reserved.

Reuse of hazardous calcium fluoride sludge from the integrated circuit industry.

PubMed

Zhu, Ping; Cao, Zhenbang; Ye, YiLi; Qian, Guangren; Lu, Bo; Zhou, Ming; Zhou, Jin

2013-11-01

The Chinese integrated circuit industry has been transformed from a small state-owned sector into a global competitor, but chip manufacturing produces large amounts of calcium fluoride sludges (CFS). In China, landfill is a current option for treating CFS. In order to solve the problem of unavailable landfill sites and prevent fluorine from dissolved CFS polluting water sources, CFS was tested as a component for a ceramic product made with sodium borate, sodium phosphate and waste alumina using a low-temperature sintering technology, and the effects of various factors on characteristics of the ceramic were investigated to optimize the process. The best sintering temperature was controlled at 700°C, and the optimal raw material ratio of the ceramic was 11% sodium borate, 54% sodium phosphate, 30% CFS and 5% waste alumina. The CFS ceramic was characterized by a morphological structure and X-ray diffraction. The results indicated that CFS was transformed into Na2Ca(PO4)F as an inert and a main crystalline phase in the ceramic, which was enclosed by the borophosphate glass. Toxicity characteristic leaching procedure, corrosion resistance and compressive strength tests verified CFS ceramic as a qualified construction ceramic material, and the fluorine from CFS was solidified in the inert crystalline phase, which would not be released to cause secondary pollution. This novel technology not only avoids the CFS hydrolyzing reaction forming harmful hydrofluoric acid gas at 800°C and above, but also produces high-performance ceramics as a construction material, in accordance with the concept of sustainable development.

Structure and short time degradation studies of sodium zirconium phosphate ceramics loaded with simulated fast breeder (FBR) waste

NASA Astrophysics Data System (ADS)

Ananthanarayanan, A.; Ambashta, R. D.; Sudarsan, V.; Ajithkumar, T.; Sen, D.; Mazumder, S.; Wattal, P. K.

2017-04-01

Sodium zirconium phosphate (NZP) ceramics have been prepared using conventional sintering and hot isostatic pressing (HIP) routes. The structure of NZP ceramics, prepared using the HIP route, has been compared with conventionally sintered NZP using a combination of X-ray diffraction (XRD) and (31P and 23Na) nuclear magnetic resonance (NMR) spectroscopy techniques. It is observed that NZP with no waste loading is aggressive toward the steel HIP-can during hot isostatic compaction and significant fraction of cations from the steel enter the ceramic material. Waste loaded NZP samples (10 wt% simulated FBR waste) show significantly low can-interaction and primary NZP phase is evident in this material. Upon exposure of can-interacted and waste loaded NZP to boiling water and steam, 31P NMR does not detect any major modifications in the network structure. However, the 23Na NMR spectra indicate migration of Na+ ions from the surface and possible re-crystallization. This is corroborated by Small-Angle Neutron Scattering (SANS) data and Scanning Electron Microscopy (SEM) measurements carried out on these samples.

The performance of biological anaerobic filters packed with sludge-fly ash ceramic particles (SFCP) and commercial ceramic particles (CCP) during the restart period: effect of the C/N ratios and filter media.

PubMed

Yue, Qinyan; Han, Shuxin; Yue, Min; Gao, Baoyu; Li, Qian; Yu, Hui; Zhao, Yaqin; Qi, Yuanfeng

2009-11-01

Two lab-scale upflow biological anaerobic filters (BAF) packed with sludge-fly ash ceramic particles (SFCP) and commercial ceramic particles (CCP) were employed to investigate effects of the C/N ratios and filter media on the BAF performance during the restart period. The results indicated that BAF could be restarted normally after one-month cease. The C/N ratio of 4.0 was the thresholds of nitrate removal and nitrite accumulation. TN removal and phosphate uptake reached the maximum value at the same C/N ratio of 5.5. Ammonia formation was also found and excreted a negative influence on TN removal, especially when higher C/N ratios were applied. Nutrients were mainly degraded within the height of 25 cm from the bottom. In addition, SFCP, as novel filter media manufactured by wastes-dewatered sludge and fly ash, represented a better potential in inhibiting nitrite accumulation, TN removal and phosphate uptake due to their special characteristics in comparison with CCP.

Phase assemblage study and cytocompatibility property of heat treated potassium magnesium phosphate-silicate ceramics.

PubMed

Kumar, Ravi; Kalmodia, Sushma; Nath, Shekhar; Singh, Dileep; Basu, Bikramjit

2009-08-01

This article reports the study on a new generation bioactive ceramic, based on MgKPO(4) (Magnesium Potassium Phosphate, abbreviated as MKP) for biomedical applications. A series of heat treatment experiments on the slip cast silica (SiO(2)) containing MKP ceramics were carried out at 900, 1,000 and 1,100 degrees C for 4 h in air. The density of the slip cast ceramic increases to 2.5 gm/cm(3) upon heat treatment at 900 degrees C. However, no significant change in density is measured upon heat treatment to higher temperature of 1,000 and 1,100 degrees C. On the basis of XRD results, the presence of K(2)MgSi(5)O(12) and dehydrated MgKPO(4) were confirmed and complementary information has also been obtained using FT-IR and Raman spectroscopy. In order to confirm the in vitro cytocompatibility property, the cell culture tests were carried out on selected samples and the results reveal good cell adhesion and spreading of L929 mouse fibroblast cells. MTT assay analysis with L929 cells confirmed non-cytotoxic behavior of MKP containing ceramics and the results are comparable with sintered HAp ceramics. It is expected that the newly developed MKP based materials could be a good substitute for hydroxyapatite (HAp or HA) based bioceramics.

Method and product for phosphosilicate slurry for use in dentistry and related bone cements

DOEpatents

Wagh, Arun S.; Primus, Carolyn

2006-08-01

The present invention is directed to magnesium phosphate ceramics and their methods of manufacture. The composition of the invention is produced by combining a mixture of a substantially dry powder component with a liquid component. The substantially dry powder component comprises a sparsely soluble oxide powder, an alkali metal phosphate powder, a sparsely soluble silicate powder, with the balance of the substantially dry powder component comprising at least one powder selected from the group consisting of bioactive powders, biocompatible powders, fluorescent powders, fluoride releasing powders, and radiopaque powders. The liquid component comprises a pH modifying agent, a monovalent alkali metal phosphate in aqueous solution, the balance of the liquid component being water. The use of calcined magnesium oxide as the oxide powder and hydroxylapatite as the bioactive powder produces a self-setting ceramic that is particularly suited for use in dental and orthopedic applications.

Bioactivity of calcium phosphate bioceramic coating fabricated by laser cladding

NASA Astrophysics Data System (ADS)

Zhu, Yizhi; Liu, Qibin; Xu, Peng; Li, Long; Jiang, Haibing; Bai, Yang

2016-05-01

There were always strong expectations for suitable biomaterials used for bone regeneration. In this study, to improve the biocompatiblity of titanium alloy, calcium phosphate bioceramic coating was obtained by laser cladding technology. The microstructure, phases, bioactivity, cell differentiation, morphology and resorption lacunae were investigated by optical microscope (OM), x-ray diffraction (XRD), methyl thiazolyl tetrazolium (MTT) assay, tartrate-resistant acid phosphatase (TRAP) staining and scanning electronic microscope (SEM), respectively. The results show that bioceramic coating consists of three layers, which are a substrate, an alloyed layer and a ceramic layer. Bioactive phases of β-tricalcium phosphate (β-TCP) and hydroxyapatite (HA) were found in ceramic coating. Osteoclast precursors have excellent proliferation on the bioceramic surface. The bioceramics coating could be digested by osteoclasts, which led to the resorption lacunae formed on its surface. It revealed that the gradient bioceramic coating has an excellent bioactivity.

Materials processing in space bibliography, 1983, revised

NASA Technical Reports Server (NTRS)

Pentecost, E. (Compiler)

1983-01-01

Flight experiments utilizing a low gravity environment to elucidate and control various processes, or ground based activities that provide supporting research are compiled. Six major categories: crystal growth; solidification of metals, alloys, and composites; fluids, transports, and chemical processes; glasses and ceramics; ultrahigh vacuum and containerless processing technologies; and combustion are included. A list of patents and appendices providing a compilation of anonymously authored collections and reports and a cross reference index are included.

Effects of different production technologies on mechanical and metallurgical properties of precious metal denture alloys

NASA Astrophysics Data System (ADS)

Ferro, Paolo; Battaglia, Eleonora; Capuzzi, Stefano; Berto, Filippo

2017-12-01

Precious metal alloys can be supplied in traditional plate form or innovative drop form with high degree of purity. The aim of the present work is to evaluate the influence of precious metal alloy form on metallurgical and mechanical properties of the final dental products with particular reference to metal-ceramic bond strength and casting defects. A widely used alloy for denture was selected; its nominal composition was close to 55 wt% Pd - 34 wt% Ag - 6 wt% In - 3 wt% Sn. Specimens were produced starting from the alloy in both plate and drop forms. A specific test method was developed to obtain results that could be representative of the real conditions of use. In order to achieve further information about the adhesion behaviour and resistance, the fracture surfaces of the samples were observed using `Scanning Electron Microscopy (SEM)'. Moreover, material defects caused by the moulding process were studied. The form of the alloy before casting does not significantly influence the shear bond strength between the metal and the ceramic material (p-value=0,976); however, according to SEM images, products from drop form alloy show less solidification defects compared to products obtained with plate form alloy. This was attributed to the absence of polluting additives used in the production of drop form alloy. This study shows that the use of precious metal denture alloys supplied in drop form does not affect the metal-ceramic bond strength compared to alloys supplied in the traditional plate form. However, compared to the plate form, the drop form is found free of solidification defects, less expensive to produce and characterized by minor environmental impacts.

Comparative study on in vitro biocompatibility of synthetic octacalcium phosphate and calcium phosphate ceramics used clinically.

PubMed

Morimoto, Shinji; Anada, Takahisa; Honda, Yoshitomo; Suzuki, Osamu

2012-08-01

The present study was designed to investigate the extent to which calcium phosphate bone substitute materials, including osteoconductive octacalcium phosphate (OCP), display cytotoxic and inflammatory responses based on their dissolution in vitro. Hydroxyapatite (HA) and β-tricalcium phosphate (β-TCP) ceramics, which are clinically used, as well as dicalcium phosphate dihydrate (DCPD) and synthesized OCP were compared. The materials were well characterized by chemical analysis, x-ray diffraction and Fourier transform infrared spectroscopy. Calcium and phosphate ion concentrations and the pH of culture media after immersion of the materials were determined. The colony forming rate of Chinese hamster lung fibroblasts was estimated with extraction of the materials. Proliferation of bone marrow stromal ST-2 cells and inflammatory cytokine TNF-α production by THP-1 cells grown on the material-coated plates were examined. The materials had characteristics that corresponded to those reported. DCPD was shown to dissolve the most in the culture media, with a marked increase in phosphate ion concentration and a reduction in pH. ST-2 cells proliferated well on the materials, with the exception of DCPD, which markedly inhibited cellular growth. The colony forming capacity was the lowest on DCPD, while that of the other calcium phosphates was not altered. In contrast, TNF-α was not detected even in cells grown on DCPD, suggesting that calcium phosphate materials are essentially non-inflammatory, while the solubility of the materials can affect osteoblastic and fibroblastic cellular attachment. These results indicate that OCP is biocompatible, which is similar to the materials used clinically, such as HA. Therefore, OCP could be clinically used as a biocompatible bone substitute material.

Formulating Precursors for Coating Metals and Ceramics

NASA Technical Reports Server (NTRS)

Morales, Wilfredo; Gatica, Jorge E.; Reye, John T.

2005-01-01

A protocol has been devised for formulating low-vapor-pressure precursors for protective and conversion coatings on metallic and ceramic substrates. The ingredients of a precursor to which the protocol applies include additives with phosphate esters, or aryl phosphate esters in solution. Additives can include iron, chromium, and/or other transition metals. Alternative or additional additives can include magnesium compounds to facilitate growth of films on substrates that do not contain magnesium. Formulation of a precursor begins with mixing of the ingredients into a high-vapor-pressure solvent to form a homogeneous solution. Then the solvent is extracted from the solution by evaporation - aided, if necessary, by vacuum and/or slight heating. The solvent is deemed to be completely extracted when the viscosity of the remaining solution closely resembles the viscosity of the phosphate ester or aryl phosphate ester. In addition, satisfactory removal of the solvent can be verified by means of a differential scanning calorimetry essay: the absence of endothermic processes for temperatures below 150 C would indicate that the residual solvent has been eliminated from the solution beyond a detectable dilution level.

High temperature furnace modeling and performance verifications

NASA Technical Reports Server (NTRS)

Smith, James E., Jr.

1992-01-01

Analytical, numerical, and experimental studies were performed on two classes of high temperature materials processing sources for their potential use as directional solidification furnaces. The research concentrated on a commercially available high temperature furnace using a zirconia ceramic tube as the heating element and an Arc Furnace based on a tube welder. The first objective was to assemble the zirconia furnace and construct parts needed to successfully perform experiments. The 2nd objective was to evaluate the zirconia furnace performance as a directional solidification furnace element. The 3rd objective was to establish a data base on materials used in the furnace construction, with particular emphasis on emissivities, transmissivities, and absorptivities as functions of wavelength and temperature. A 1-D and 2-D spectral radiation heat transfer model was developed for comparison with standard modeling techniques, and were used to predict wall and crucible temperatures. The 4th objective addressed the development of a SINDA model for the Arc Furnace and was used to design sample holders and to estimate cooling media temperatures for the steady state operation of the furnace. And, the 5th objective addressed the initial performance evaluation of the Arc Furnace and associated equipment for directional solidification. Results of these objectives are presented.

Influence of a cellulosic ether carrier on the structure of biphasic calcium phosphate ceramic particles in an injectable composite material.

PubMed

Dupraz, A; Nguyen, T P; Richard, M; Daculsi, G; Passuti, N

1999-04-01

An injectable composite material based on biphasic calcium phosphate (BCP) and a nonionic cellulose ether has been elaborated for use in percutaneous surgery for spine fusion. This paper reports the characterization results of this material by spectroscopic techniques including X-ray diffraction (XRD), infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) fitted with an energy dispersive X-Ray analysis system and high-resolution transmission electron microscopy (HR-TEM). From FTIR and XPS results, it was observed that the adhesion between the polymer and the ceramic might be insured by oxygen bridging developed through an ionic bonding between calcium ions and (C-O) groups of the polymer. Moreover, XPS showed attraction of Ca2+ ions in the polymer matrix, while the ceramic surface was modified in a HPO4(2-) -rich layer. These results suggest a possible dissolution/precipitation process at the interface ceramic/polymer. HR-TEM observations supported this hypothesis, showing a light contrasted fringe at the surface of the ceramic grains in the composite paste. As well, changes in the XRD spectra could indicate a small decrease in the crystal size of the BCP powder through the contact to polymer solution. In addition, SEM observation showed a decrease of the initial BCP granulometry. Aggregates of 80-200 microm seemed to be mostly dissociated in micrograins. The ceramic grains were coated with and bonded between each other by the polymer matrix, which acted as spacer in between the ceramic grains, creating a macroporous-like material structure.

Silicon-on ceramic process: Silicon sheet growth and device development for the large-area silicon sheet task of the low-cost solar array project

NASA Technical Reports Server (NTRS)

Grung, B. L.; Heaps, J. D.; Schmit, F. M.; Schuldt, S. B.; Zook, J. D.

1981-01-01

The technical feasibility of producing solar-cell-quality sheet silicon to meet the Department of Energy (DOE) 1986 overall price goal of $0.70/watt was investigated. With the silicon-on-ceramic (SOC) approach, a low-cost ceramic substrate is coated with large-grain polycrystalline silicon by unidirectional solidification of molten silicon. This effort was divided into several areas of investigation in order to most efficiently meet the goals of the program. These areas include: (1) dip-coating; (2) continuous coating designated SCIM-coating, and acronym for Silicon Coating by an Inverted Meniscus (SCIM); (3) material characterization; (4) cell fabrication and evaluation; and (5) theoretical analysis. Both coating approaches were successful in producing thin layers of large grain, solar-cell-quality silicon. The dip-coating approach was initially investigated and considerable effort was given to this technique. The SCIM technique was adopted because of its scale-up potential and its capability to produce more conventiently large areas of SOC.

Continuous coating of silicon-on-ceramic

NASA Technical Reports Server (NTRS)

Heaps, J. D.; Schuldt, S. B.; Grung, B. L.; Zook, J. D.; Butter, C. D.

1980-01-01

Growth of sheet silicon on low-cost substrates has been demonstrated by the silicon coating with inverted meniscus (SCIM) technique. A mullite-based ceramic substrate is coated with carbon and then passed over a trough of molten silicon with a raised meniscus. Solidification occurs at the trailing edge of the downstream meniscus, producing a silicon-on-ceramic (SOC) layer. Meniscus shape and stability are controlled by varying the level of molten silicon in a reservoir connected to the trough. The thermal conditions for growth and the crystallographic texture of the SOC layers are similar to those produced by dip-coating, the original technique of meniscus-controlled growth. The thermal conditions for growth have been analyzed in some detail. The analysis correctly predicts the velocity-thickness relationship and the liquid-solid interface shape for dip-coating, and appears to be equally applicable to SCIM-coating. Solar cells made from dip-coated SOC material have demonstrated efficiencies of 10% on 4-sq cm cells and 9.9% on 10-sq cm cells.

Use of high temperature insulation for ceramic matrix composites in gas turbines

DOEpatents

Morrison, Jay Alan; Merrill, Gary Brian; Ludeman, Evan McNeil; Lane, Jay Edgar

2001-01-01

A ceramic composition for insulating components, made of ceramic matrix composites, of gas turbines is provided. The composition comprises a plurality of hollow oxide-based spheres of various dimensions, a phosphate binder, and at least one oxide filler powder, whereby the phosphate binder partially fills gaps between the spheres and the filler powders. The spheres are situated in the phosphate binder and the filler powders such that each sphere is in contact with at least one other sphere and the arrangement of spheres is such that the composition is dimensionally stable and chemically stable at a temperature of approximately 1600.degree. C. A stationary vane of a gas turbine comprising the composition of the present invention bonded to the outer surface of the vane is provided. A combustor comprising the composition bonded to the inner surface of the combustor is provided. A transition duct comprising the insulating coating bonded to the inner surface of the transition is provided. Because of abradable properties of the composition, a gas turbine blade tip seal comprising the composition also is provided. The composition is bonded to the inside surface of a shroud so that a blade tip carves grooves in the composition so as to create a customized seal for the turbine blade tip.

β-tricalcium phosphate composite ceramics with high compressive strength, enhanced osteogenesis and inhibited osteoclastic activities.

PubMed

Tian, Ye; Lu, Teliang; He, Fupo; Xu, Yubin; Shi, Haishan; Shi, Xuetao; Zuo, Fei; Wu, Shanghua; Ye, Jiandong

2018-04-13

β-tricalcium phosphate (β-TCP) is well known as a resorbable bone repair material due to its inherent excellent biocompatibility and osteoconductivity. However, β-TCP is encountered with osteostimulation-deficiency and poor mechanical strength because of poor sinterability. Herein, we prepared novel β-TCP composite ceramics (TCP/SPGs) by introducing strontium-containing phosphate-based glass (SPG; 45P 2 O 5 -32SrO-23Na 2 O) as sintering additive. The SPG helped to achieve efficient liquid-phase sintering of β-TCP at 1100 °C. The compressive strength of TCP/SPGs with 15 wt.% SPG (TCP/SPG15) was 2.65 times as high as that of plain β-TCP ceramic. The SPG reacted with β-TCP, and the Sr 2+ and Na 2+ from SPG replaced Ca 2+ in the lattice structure of β-TCP, enabling the sustained release of strontium from TCP/SPGs. In vitro cytological test indicated that TCP/SPGs with certain amount of SPG were highly biocompatible, and noticeably promoted osteogenesis, and inhibited osteoclastic activities. Our results suggested that the TCP/SPG15 might be potential high-strength bone grafts used for bone defect repair, especially in the osteoporotic condition. Copyright © 2018 Elsevier B.V. All rights reserved.

Method of waste stabilization with dewatered chemically bonded phosphate ceramics

DOEpatents

Wagh, Arun; Maloney, Martin D.

2010-06-29

A method of stabilizing a waste in a chemically bonded phosphate ceramic (CBPC). The method consists of preparing a slurry including the waste, water, an oxide binder, and a phosphate binder. The slurry is then allowed to cure to a solid, hydrated CBPC matrix. Next, bound water within the solid, hydrated CBPC matrix is removed. Typically, the bound water is removed by applying heat to the cured CBPC matrix. Preferably, the quantity of heat applied to the cured CBPC matrix is sufficient to drive off water bound within the hydrated CBPC matrix, but not to volatalize other non-water components of the matrix, such as metals and radioactive components. Typically, a temperature range of between 100.degree. C.-200.degree. C. will be sufficient. In another embodiment of the invention wherein the waste and water have been mixed prior to the preparation of the slurry, a select amount of water may be evaporated from the waste and water mixture prior to preparation of the slurry. Another aspect of the invention is a direct anyhydrous CBPC fabrication method wherein water is removed from the slurry by heating and mixing the slurry while allowing the slurry to cure. Additional aspects of the invention are ceramic matrix waste forms prepared by the methods disclosed above.

Tensile Bond Strength of So-called Universal Primers and Universal Multimode Adhesives to Zirconia and Lithium Disilicate Ceramics.

PubMed

Elsayed, Adham; Younes, Feras; Lehmann, Frank; Kern, Matthias

2017-01-01

To test the bond strength and durability after artificial aging of so-called universal primers and universal multimode adhesives to lithium disilicate or zirconia ceramics. A total of 240 ceramic plates, divided into two groups, were produced and conditioned: 120 acid-etched lithium disilicate plates (IPS e.max CAD) and 120 air-abraded zirconia plates (Zenostar T). Each group was divided into five subgroups (n = 24), and a universal restorative primer or multimode universal adhesive was used for each subgroup to bond plexiglas tubes filled with a composite resin to the ceramic plate. The specimens were stored in water at 37°C for 3 days without thermal cycling, or for 30 or 150 days with 7500 or 37,500 thermal cycles between 5°C and 55°C, respectively. All specimens then underwent tensile bond strength testing. Initially, all bonding systems exhibited high TBS, but some showed a significant reduction after 30 and 150 days of storage. After 3, 30, and 150 days, Monobond Plus, which contains silane and phosphate monomer, showed significantly higher bond strengths than the other universal primer and adhesive systems. The bond strength to lithium disilicate and zirconia ceramic is significantly affected by the bonding system used. Using a separate primer containg silane and phosphate monomer provides more durable bonding than do silanes incorporated in universal multimode adhesives. Only one of five so-called universal primers and adhesives provided durable bonding to lithium disilicate and zirconia ceramic.

Epitaxial Growth and Cracking Mechanisms of Thermally Sprayed Ceramic Splats

NASA Astrophysics Data System (ADS)

Chen, Lin; Yang, Guan-jun

2018-02-01

In the present study, the epitaxial growth and cracking mechanisms of thermally sprayed ceramic splats were explored. We report, for the first time, the epitaxial growth of various splat/substrate combinations at low substrate temperatures (100 °C) and large lattice mismatch (- 11.26%). Our results suggest that thermal spray deposition was essentially a liquid-phase epitaxy, readily forming chemical bonding. The interface temperature was also estimated. The results convincingly demonstrated that atoms only need to diffuse and rearrange over a sufficiently short range during extremely rapid solidification. Concurrently, severe cracking occurred in the epitaxial splat/substrate systems, which indicated high tensile stress was produced during splat deposition. The origin of the tensile stress was attributed to the strong constraint of the locally heated substrate by its cold surroundings.

Inverse liquid chromatography as a tool for characterisation of the surface layer of ceramic biomaterials.

PubMed

Kadlec, Karol; Adamska, Katarzyna; Okulus, Zuzanna; Voelkel, Adam

2016-10-14

The novel technique for ceramic biomaterials surface characterisation was proposed. The examined bone substitute materials were two orthophosphates: hydroxyapatite, β-tricalcium phosphate and the mixture of these two - biphasic calcium phosphate. The aim of this work was characterisation of the ceramic biomaterials surface expressed via the values of parameters e, s, a, b, v considered in linear free energy relationship. The values of these parameters reflect the ability of stationary phase to occur in different types of interactions. The sorption phenomena occurring on the bone substitute materials surface are responsible for the process of the multiplication of the osteoblasts. Thus the detailed description of this phenomena may contribute to the better understanding of bone loss regeneration mechanism. The data required for characterisation by using LFER model was collected by means of inverse liquid chromatography with the use of five different mobile phases: 98% ethanol, ethanol/water (50/50), water, 0.2M NaCl and SBF. The determination of the ceramic orthophosphates surface properties in SBF solution allowed to observe the behaviour of biomaterials in "natural environment" - in living organism. Copyright © 2016 Elsevier B.V. All rights reserved.

Topography of calcium phosphate ceramics regulates primary cilia length and TGF receptor recruitment associated with osteogenesis.

PubMed

Zhang, Jingwei; Dalbay, Melis T; Luo, Xiaoman; Vrij, Erik; Barbieri, Davide; Moroni, Lorenzo; de Bruijn, Joost D; van Blitterswijk, Clemens A; Chapple, J Paul; Knight, Martin M; Yuan, Huipin

2017-07-15

The surface topography of synthetic biomaterials is known to play a role in material-driven osteogenesis. Recent studies show that TGFβ signalling also initiates osteogenic differentiation. TGFβ signalling requires the recruitment of TGFβ receptors (TGFβR) to the primary cilia. In this study, we hypothesize that the surface topography of calcium phosphate ceramics regulates stem cell morphology, primary cilia structure and TGFβR recruitment to the cilium associated with osteogenic differentiation. We developed a 2D system using two types of tricalcium phosphate (TCP) ceramic discs with identical chemistry. One sample had a surface topography at micron-scale (TCP-B, with a bigger surface structure dimension) whilst the other had a surface topography at submicron scale (TCP-S, with a smaller surface structure dimension). In the absence of osteogenic differentiation factors, human bone marrow stromal cells (hBMSCs) were more spread on TCP-S than on TCP-B with alterations in actin organization and increased primary cilia prevalence and length. The cilia elongation on TCP-S was similar to that observed on glass in the presence of osteogenic media and was followed by recruitment of transforming growth factor-β RII (p-TGFβ RII) to the cilia axoneme. This was associated with enhanced osteogenic differentiation of hBMSCs on TCP-S, as shown by alkaline phosphatase activity and gene expression for key osteogenic markers in the absence of additional osteogenic growth factors. Similarly, in vivo after a 12-week intramuscular implantation in dogs, TCP-S induced bone formation while TCP-B did not. It is most likely that the surface topography of calcium phosphate ceramics regulates primary cilia length and ciliary recruitment of p-TGFβ RII associated with osteogenesis and bone formation. This bioengineering control of osteogenesis via primary cilia modulation may represent a new type of biomaterial-based ciliotherapy for orthopedic, dental and maxillofacial surgery applications. The surface topography of synthetic biomaterials plays important roles in material-driven osteogenesis. The data presented herein have shown that the surface topography of calcium phosphate ceramics regulates mesenchymal stromal cells (e.g., human bone marrow mesenchymal stromal cells, hBMSCs) with respect to morphology, primary cilia structure and TGFβR recruitment to the cilium associated with osteogenic differentiation in vitro. Together with bone formation in vivo, our results suggested a new type of biomaterial-based ciliotherapy for orthopedic, dental and maxillofacial surgery by the bioengineering control of osteogenesis via primary cilia modulation. Copyright © 2017 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

The effect of water-soluble polymers on the microstructure and properties of freeze-cast alumina ceramics

NASA Astrophysics Data System (ADS)

Pekor, Christopher Michael

Porous ceramics can be divided into three separate classes based on their pore size: microporous ceramics with pores less than 2 nm, mesoporous ceramics with pores in the range of 2--50 nm and macroporous ceramics with pores that are greater than 50 nm. In particular, macroporous ceramics are used in a variety of applications such as refractories, molten metal filtration, diesel particulate filters, heterogeneous catalyst supports and biomedical scaffolds. Freeze casting is a novel method used to create macroporous ceramics. In this method growing ice crystals act as a template for the pores and are solidified, often directionally, through a ceramic dispersion and removed from the green body through a freeze drying procedure. This method has attracted some attention over the past few years due to its relative simplicity, flexibility and environmental friendliness. On top of this freeze casting is capable of producing materials with high pore volume fractions, which is an advantage over processing by packing and necking of particles, where the pore volume fraction is typically less than 50%. Many of the basic processing variables that affect the freeze cast microstructure, such as the temperature gradient, interfacial velocity and solid loading of the dispersion have been well established in the literature. On the other hand, areas such as the effect of additives on the microstructure and mechanical properties have not been covered in great detail. In this study the concept of constitutional supercooling from basic solidification theory is used to explain the effects of two water-soluble polymers, polyethylene glycol and polyvinyl alcohol, on the microstructure of freeze cast alumina ceramics. In addition, changes in the observed microstructure will be related to experimentally determined values of permeability and compressive strength.

The ultrastructure and processing properties of Straumann Bone Ceramic and NanoBone.

PubMed

Dietze, S; Bayerlein, T; Proff, P; Hoffmann, A; Gedrange, T

2006-02-01

The ultrastructure, fundamental chemistry, and processing modes of fully synthetic bone grafting materials are relevant to the reconstruction of osseous defects. Rapid progress in the profitable market of biomaterials has led to the development of various bone substitutes. Despite all these efforts, an ideal and full substitute of autologous bone is not yet in sight. With regard to anorganic calcium phosphate ceramics, Straumann Bone Ceramic and NanoBone are compared. These have a similar composition and are osteoconductive, which indispensably requires contact with well-vascularised bone.

Influence of polarized PZT on the crystal growth of calcium phosphate

NASA Astrophysics Data System (ADS)

Sun, Xiaodan; Ma, Chunlai; Wang, Yude; Li, Hengde

2002-01-01

The effects of polarization on the crystallization of calcium phosphate are studied in this work. Crystals of calcium phosphate from saturated solution of hydroxyapatite (HA, Ca 10(PO 4) 6(OH) 2) were deposited on the surfaces of ferroelectric ceramics lead zirconate titanium (Pb(Ti,Zr)O 3, PZT). The results of the experiment demonstrated the acceleration effects of polarized PZT on the crystal growth of calcium phosphate. Furthermore, it is indicated that polarization also influenced the orientation of the deposited crystals due to the growth of a layer of (0 0 2) oriented octacalcium phosphate (OCP, Ca 8H 2(PO 4) 6·5H 2O) on the negatively charged surfaces of PZT.

An Investigation of Fiber Reinforced Chemically Bonded Phosphate Ceramic Composites at Room Temperature.

PubMed

Ding, Zhu; Li, Yu-Yu; Lu, Can; Liu, Jian

2018-05-21

In this study, chemically bonded phosphate ceramic (CBPC) fiber reinforced composites were made at indoor temperatures. The mechanical properties and microstructure of the CBPC composites were studied. The CBPC matrix of aluminum phosphate binder, metakaolin, and magnesia with different Si/P ratios was prepared. The results show that when the Si/P ratio was 1.2, and magnesia content in the CBPC was 15%, CBPC reached its maximum flexural strength. The fiber reinforced CBPC composites were prepared by mixing short polyvinyl alcohol (PVA) fibers or unidirectional continuous carbon fiber sheets. Flexural strength and dynamic mechanical properties of the composites were determined, and the microstructures of specimens were analyzed by scanning electron micrography, X-ray diffraction, and micro X-ray computed tomography. The flexural performance of continuous carbon fiber reinforced CBPC composites was better than that of PVA fiber composites. The elastic modulus, loss modulus, and loss factor of the fiber composites were measured through dynamic mechanical analysis. The results showed that fiber reinforced CBPC composites are an inorganic polymer viscoelastic material with excellent damping properties. The reaction of magnesia and phosphate in the matrix of CBPC formed a different mineral, newberyite, which was beneficial to the development of the CBPC.

Interaction mechanisms between ceramic particles and atomized metallic droplets

NASA Astrophysics Data System (ADS)

Wu, Yue; Lavernia, Enrique J.

1992-10-01

The present study was undertaken to provide insight into the dynamic interactions that occur when ceramic particles are placed in intimate contact with a metallic matrix undergoing a phase change. To that effect, Al-4 wt pct Si/SiCp composite droplets were synthesized using a spray atomization and coinjection approach, and their solidification microstructures were studied both qualitatively and quantitatively. The present results show that SiC particles (SiCp) were incor- porated into the matrix and that the extent of incorporation depends on the solidification con- dition of the droplets at the moment of SiC particle injection. Two factors were found to affect the distribution and volume fraction of SiC particles in droplets: the penetration of particles into droplets and the entrapment and/or rejection of particles by the solidification front. First, during coinjection, particles collide with the atomized droplets with three possible results: they may penetrate the droplets, adhere to the droplet surface, or bounce back after impact. The extent of penetration of SiC particles into droplets was noted to depend on the kinetic energy of the particles and the magnitude of the surface energy change in the droplets that occurs upon impact. In liquid droplets, the extent of penetration of SiC particles was shown to depend on the changes in surface energy, ΔEs, experienced by the droplets. Accordingly, large SiC particles encoun- tered more resistance to penetration relative to small ones. In solid droplets, the penetration of SiC particles was correlated with the dynamic pressure exerted by the SiC particles on the droplets during impact and the depth of the ensuing crater. The results showed that no pene- tration was possible in such droplets. Second, once SiC particles have penetrated droplets, their final location in the microstructure is governed by their interactions with the solidification front. As a result of these interactions, both entrapment and rejection of SiC particles occurred during droplet solidification. A comparison of the present results to those anticipated from well-established kinetic and thermodynamic models led to some interesting findings. First, the models proposed by Boiling and Cisse[24] and Chernov et al.[58] predict relative low critical interface velocities necessary for entrapment, inconsistent with the present experimental findings. Second, although the observed correlation between the critical front velocity and droplet diameter was generally consistent with that predicted by Stefanescu et a/.’s model,[27] the dependence on the size of SiC particles was not. In view of this discrepancy, three possible mechanisms were proposed to account for the experimental findings: nucleation of α-Al on SiC particles, entrapment of SiC particles between primary dendrite arms, and entrapment of SiC particles between secondary dendrite arms.

Interlaboratory studies on in vitro test methods for estimating in vivo resorption of calcium phosphate ceramics.

PubMed

Ito, Atsuo; Sogo, Yu; Yamazaki, Atsushi; Aizawa, Mamoru; Osaka, Akiyoshi; Hayakawa, Satoshi; Kikuchi, Masanori; Yamashita, Kimihiro; Tanaka, Yumi; Tadokoro, Mika; de Sena, Lídia Ágata; Buchanan, Fraser; Ohgushi, Hajime; Bohner, Marc

2015-10-01

A potential standard method for measuring the relative dissolution rate to estimate the resorbability of calcium-phosphate-based ceramics is proposed. Tricalcium phosphate (TCP), magnesium-substituted TCP (MgTCP) and zinc-substituted TCP (ZnTCP) were dissolved in a buffer solution free of calcium and phosphate ions at pH 4.0, 5.5 or 7.3 at nine research centers. Relative values of the initial dissolution rate (relative dissolution rates) were in good agreement among the centers. The relative dissolution rate coincided with the relative volume of resorption pits of ZnTCP in vitro. The relative dissolution rate coincided with the relative resorbed volume in vivo in the case of comparison between microporous MgTCPs with different Mg contents and similar porosity. However, the relative dissolution rate was in poor agreement with the relative resorbed volume in vivo in the case of comparison between microporous TCP and MgTCP due to the superimposition of the Mg-mediated decrease in TCP solubility on the Mg-mediated increase in the amount of resorption. An unambiguous conclusion could not be made as to whether the relative dissolution rate is predictive of the relative resorbed volume in vivo in the case of comparison between TCPs with different porosity. The relative dissolution rate may be useful for predicting the relative amount of resorption for calcium-phosphate-based ceramics having different solubility under the condition that the differences in the materials compared have little impact on the resorption process such as the number and activity of resorbing cells. The evaluation and subsequent optimization of the resorbability of calcium phosphate are crucial in the use of resorbable calcium phosphates. Although the resorbability of calcium phosphates has usually been evaluated in vivo, establishment of a standard in vitro method that can predict in vivo resorption is beneficial for accelerating development and commercialization of new resorbable calcium phosphate materials as well as reducing use of animals. However, there are only a few studies to propose such an in vitro method within which direct comparison was carried out between in vitro and in vivo resorption. We propose here an in vitro method based on measuring dissolution rate. The efficacy and limitations of the method were evaluated by international round-robin tests as well as comparison with in vivo resorption studies for future standardization. This study was carried out as one of Versailles Projects on Advanced Materials and Standards (VAMAS). Copyright © 2015 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Enhanced In Vivo Bone and Blood Vessel Formation by Iron Oxide and Silica Doped 3D Printed Tricalcium Phosphate Scaffolds.

PubMed

Bose, Susmita; Banerjee, Dishary; Robertson, Samuel; Vahabzadeh, Sahar

2018-05-04

Calcium phosphate (CaP) ceramics show significant promise towards bone graft applications because of the compositional similarity to inorganic materials of bone. With 3D printing, it is possible to create ceramic implants that closely mimic the geometry of human bone and can be custom-designed for unusual injuries or anatomical sites. The objective of the study was to optimize the 3D-printing parameters for the fabrication of scaffolds, with complex geometry, made from synthesized tricalcium phosphate (TCP) powder. This study was also intended to elucidate the mechanical and biological effects of the addition of Fe +3 and Si +4 in TCP implants in a rat distal femur model for 4, 8, and 12 weeks. Doped with Fe +3 and Si +4 TCP scaffolds with 3D interconnected channels were fabricated to provide channels for micronutrients delivery and improved cell-material interactions through bioactive fixation. Addition of Fe +3 into TCP enhanced early-stage new bone formation by increasing type I collagen production. Neovascularization was observed in the Si +4 doped samples after 12 weeks. These findings emphasize that the additive manufacturing of scaffolds with complex geometry from synthesized ceramic powder with modified chemistry is feasible and may serve as a potential candidate to introduce angiogenic and osteogenic properties to CaPs, leading to accelerated bone defect healing.

[Microstructure and mechanical property of a new IPS-Empress 2 dental glass-ceramic].

PubMed

Luo, Xiao-ping; Watts, D C; Wilson, N H F; Silsons, N; Cheng, Ya-qin

2005-03-01

To investigate the microstructure and mechanical properties of a new IPS-Empress 2 dental glass-ceramic. AFM, SEM and XRD were used to analyze the microstructure and crystal phase of IPS-Empress 2 glass-ceramic. The flexural strength and fracture toughness were tested using 3-point bending method and indentation method respectively. IPS-Empress 2 glass-ceramic mainly consisted of lithium disilicate crystal, lithium phosphate and glass matrix, which formed a continuous interlocking structure. The crystal phases were not changed before and after hot-pressed treatment. AFM showed nucleating agent particles of different sizes distributed on the highly polished ceramic surface. The strength and fracture toughness were 300 MPa and 3.1 MPam(1/2). The high strength and fracture toughness of IPS-Empress 2 glass ceramic are attributed to the fine lithium disilicate crystalline, interlocking microstructure and crack deflection.

Morphology and Shear Strength of Lead-Free Solder Joints with Sn3.0Ag0.5Cu Solder Paste Reinforced with Ceramic Nanoparticles

NASA Astrophysics Data System (ADS)

Yakymovych, A.; Plevachuk, Yu.; Švec, P.; Švec, P.; Janičkovič, D.; Šebo, P.; Beronská, N.; Roshanghias, A.; Ipser, H.

2016-12-01

To date, additions of different oxide nanoparticles is one of the most widespread procedures to improve the mechanical properties of metals and metal alloys. This research deals with the effect of minor ceramic nanoparticle additions (SiO2, TiO2 and ZrO2) on the microstructure and mechanical properties of Cu/solder/Cu joints. The reinforced Sn3.0Ag0.5Cu (SAC305) solder alloy with 0.5 wt.% and 1.0 wt.% of ceramic nanoparticles was prepared through mechanically stirring. The microstructure of as-solidified Cu/solder/Cu joints was studied using scanning electron microscopy. The additions of ceramic nanoparticles suppressed the growth of the intermetallic compound layer Cu6Sn5 at the interface solder/Cu and improved the microstructure of the joints. Furthermore, measurements of mechanical properties showed improved shear strength of Cu/composite solder/Cu joints compared to joints with unreinforced solder. This fact related to all investigated ceramic nanoinclusions and should be attributed to the adsorption of nanoparticles on the grain surface during solidification. However, this effect is less pronounced on increasing the nanoinclusion content from 0.5 wt.% to 1.0 wt.% due to agglomeration of nanoparticles. Moreover, a comparison analysis showed that the most beneficial influence was obtained by minor additions of SiO2 nanoparticles into the SAC305 solder alloy.

Ectopic bone formation cannot occur by hydroxyapatite/β-tricalcium phosphate bioceramics in green fluorescent protein chimeric mice

NASA Astrophysics Data System (ADS)

Cheng, Lijia; Duan, Xin; Xiang, Zhou; Shi, Yujun; Lu, Xiaofeng; Ye, Feng; Bu, Hong

2012-12-01

Many studies have shown that calcium phosphate ceramics (CP) have osteoconductive and osteoinductive properties; however, the exact mechanism of bone induction has not yet been reported. This study was performed to investigate if destroying immunological function will influence osteogenesis, to explain the mechanism which is unclear. In this study, twenty C57BL/6 mice were divided into two groups (n = 10), in group 1, a hydroxyapatite/β-tricalcium phosphate (HA/β-TCP) ceramic was implanted into both the left and right leg muscles of each mouse; in group 2, ten mice experienced lethal irradiation, then were injected bone marrow (BM) cells from green fluorescent protein (GFP) transgenic mice by tail veil, after bone marrow transplantation (BMT), heart, liver, spleen, lung, kidney, and muscle were harvested for biological analysis, after the GFP chimera model was established successfully, the same HA/β-TCP ceramic was implanted into both leg muscles of each mouse immediately after irradiation. 45 and 90 days after implantation, the ceramics of the two groups were harvested to perform with hematoxylin and eosin (HE) and immunohistochemistry (IHC) staining; the results showed that there was no bone formation in group 2, while new bone tissues were detected in group 1. Our findings suggest that the BM cell from GFP transgenic mice is a good biomarker and it could set a good platform for chimera model; it also shows that BM cell is one of cell resources of bone induction, and destruction of immune function will impede osteoinduction by CP. Overall, our results may shed light on clear mechanism study of bone induction in the future.

Dental-Implantate und ihre Werkstoffe

NASA Astrophysics Data System (ADS)

Newesely, Heinrich

1983-07-01

Some new trends in materials for dental implants, which also effect in the operative techniques and implant design, are described. Advantages and shortcomings of the different material types are exemplified and correlated with their bioinert resp. bioactive functions. The practical interest in metallic implants focussed in titanium resp. oxide ceramics in the ceramic field, whereas the special goal of implant research follows from the improvement of the bioactive principle with loaded calcium phosphate implants.

Evaluation of load at fracture of Procera AllCeram copings using different luting cements.

PubMed

Al-Makramani, Bandar M A; Razak, A A A; Abu-Hassan, M I

2008-02-01

The current study investigated the effect of different luting agents on the fracture resistance of Procera AllCeram copings. Six master dies were duplicated from the prepared maxillary first premolar tooth using nonprecious metal alloy (Wiron 99). Thirty copings (Procera AllCeram) of 0.6-mm thickness were manufactured. Three types of luting media were used: zinc phosphate cement (Elite), glass ionomer cement (Fuji I), and dual-cured composite resin cement (Panavia F). Ten copings were cemented with each type. Two master dies were used for each group, and each of them was used to lute five copings. All groups were cemented according to manufacturer's instructions and received a static load of 5 kg during cementation. After 24 hours of distilled water storage at 37 degrees C, the copings were vertically compressed using a universal testing machine at a crosshead speed of 1 mm/min. ANOVA revealed significant differences in the load at fracture among the three groups (p < 0.001). The fracture strength results showed that the mean fracture strength of zinc phosphate cement (Elite), glass ionomer cement (Fuji I), and resin luting cement (Panavia F) were 1091.9 N, 784.8 N, and 1953.5 N, respectively. Different luting agents have an influence on the fracture resistance of Procera AllCeram copings.

Trace element doping in calcium phosphate ceramics to Understand osteogenesis and angiogenesis

PubMed Central

Bose, Susmita; Fielding, Gary; Tarafder, Solaiman; Bandyopadhyay, Amit

2013-01-01

The general trends in synthetic bone grafting materials are shifting towards approaches that can illicit osteoinductive properties. Pharmacologics and biologics have been used in combination with calcium phosphate (CaP) ceramics, however, recently have become the target of scrutiny over the safety. The importance of trace elements in natural bone health is well documented. Ions, e.g. lithium, zinc, magnesium, manganese, silicon, strontium etc. have shown to increase osteogenesis and neovascularization. Incorporation of dopants into CaPs can provide a platform for safe and efficient delivery in clinical applications where increased bone healing is favorable. This review highlights use of trace elements in CaP biomaterials, and offers an insight into the mechanisms of how metal ions can enhance both osteogenesis and angiogenesis. PMID:24012308

Surface treatment of alumina-based ceramics using combined laser sources

NASA Astrophysics Data System (ADS)

Triantafyllidis, D.; Li, L.; Stott, F. H.

2002-01-01

Alumina-based refractory materials are extensively used as linings in incinerators and furnaces. These materials are subject to molten salt corrosion and chemical degradation because of the existence of porosity and material inhomogeneity. Efforts to improve the performance of these materials have so far concentrated mainly on the optimisation of the manufacturing processes (e.g. producing denser refractory bricks) and in-service monitoring. Laser surface treatment has also been used to improve performance. The main problem identified with laser surface treatment is solidification cracking due to the generation of very large temperature gradients. The aim of this paper is to investigate the surface modification of alumina-based ceramics by using two combined laser sources in order to control the thermal gradients and cooling rates during processing so that crack formation can be eliminated. The material under investigation is 85% alumina refractory ceramic, used as lining material in incineration plants. The surface morphology and cross-section of the treated samples are analysed using optical and scanning electron microscopy (SEM) and compared with single laser beam treated samples.

A hybrid composite system of biphasic calcium phosphate granules loaded with hyaluronic acid-gelatin hydrogel for bone regeneration.

PubMed

Faruq, Omar; Kim, Boram; Padalhin, Andrew R; Lee, Gun Hee; Lee, Byong-Taek

2017-10-01

An ideal bone substitute should be made of biocompatible materials that mimic the structure, characteristics, and functions of natural bone. Many researchers have worked on the fabrication of different bone scaffold systems including ceramic-polymer hybrid system. In the present study, we incorporated hyaluronic acid-gelatin hydrogel to micro-channeled biphasic calcium phosphate granules as a carrier to improve cell attachment and proliferation through highly interconnected porous structure. This hybrid system is composed of ceramic biphasic calcium phosphate granules measuring 1 mm in diameter with seven holes and hyaluronic acid-gelatin hydrogel. This combination of biphasic calcium phosphate and hyaluronic acid-gelatin retained suitable characteristics for bone regeneration. The resulting scaffold had a porosity of 56% with a suitable pore sizes. The mechanical strength of biphasic calcium phosphate granule increased after loading hyaluronic acid-gelatin from 4.26 ± 0.43 to 6.57 ± 0.25 MPa, which is highly recommended for cancellous bone substitution. Swelling and degradation rates decreased in the hybrid scaffold compared to hydrogel due to the presence of granules in hybrid scaffold. In vitro cytocompatibility studies were observed by preosteoblasts (MC3T3-E1) cell line and the result revealed that biphasic calcium phosphate/hyaluronic acid-gelatin significantly increased cell growth and proliferation compared to biphasic calcium phosphate granules. Analysis of micro-computed tomography data and stained tissue sections from the implanted samples showed that the hybrid scaffold had good osseointegration and better bone formation in the scaffold one and two months postimplantation. Histological section confirmed the formation of dense collagenous tissue and new bone in biphasic calcium phosphate/hyaluronic acid-gelatin scaffolds at two months. Our study demonstrated that such hybrid biphasic calcium phosphate/hyaluronic acid-gelatin scaffold is a promising system for bone regeneration.

Freeze-cast alumina pore networks: Effects of freezing conditions and dispersion medium

DOE Office of Scientific and Technical Information (OSTI.GOV)

Miller, S. M.; Xiao, X.; Faber, K. T.

Alumina ceramics were freeze-cast from water- and camphene-based slurries under varying freezing conditions and examined using X-ray computed tomography (XCT). Pore network characteristics, i.e., porosity, pore size, geometric surface area, and tortuosity, were measured from XCT reconstructions and the data were used to develop a model to predict feature size from processing conditions. Classical solidification theory was used to examine relationships between pore size, temperature gradients, and freezing front velocity. Freezing front velocity was subsequently predicted from casting conditions via the two-phase Stefan problem. Resulting models for water-based samples agreed with solidification-based theories predicting lamellar spacing of binary eutectic alloys,more » and models for camphene-based samples concurred with those for dendritic growth. Relationships between freezing conditions and geometric surface area were also modeled by considering the inverse relationship between pore size and surface area. Tortuosity was determined to be dependent primarily on the type of dispersion medium. (C) 2015 Elsevier Ltd. All rights reserved.« less

Mechanism of competitive grain growth in a curvilinear channel of crystal-sorter during the orientational solidification of nickel-based heat-resistant alloy

NASA Astrophysics Data System (ADS)

Monastyrskiy, V. P.; Pozdnyakov, A. N.; Ershov, M. Yu.; Monastyrskiy, A. V.

2017-07-01

Using numerical simulation in the ProCAST program complex, the conditions of the solidification of heat-resistant nickel alloy in curvilinear channels of a ceramic mold have been investigated. It has been shown that, in practically important cases, the vector of the temperature gradient is oriented along the axis of the curvilinear channel. In a spiral crystal selector, a cyclic change in the preferred direction of growth occurs because of the cyclic change in the direction of the vector of the temperature gradient. The fact that the vector of the temperature gradient is almost always directed along the axis of the curvilinear channel makes it possible to govern the orientation of the vector of the temperature gradient in space and, therefore, to obtain a grain with the preferred crystallographic orientation. Based on the results of this investigation, a method of the grain selection with a desired azimuthal orientation is proposed.

Air pollution control residues from waste incineration: current UK situation and assessment of alternative technologies.

PubMed

Rani, D Amutha; Boccaccini, A R; Deegan, D; Cheeseman, C R

2008-11-01

Current disposal options for APC residues in the UK and alternative treatment technologies developed world-wide have been reviewed. APC residues are currently landfilled in the UK where they undergo in situ solidification, although the future acceptability of this option is uncertain because the EU waste acceptance criteria (WAC) introduce strict limits on leaching that are difficult to achieve. Other APC residue treatment processes have been developed which are reported to reduce leaching to below relevant regulatory limits. The Ferrox process, the VKI process, the WES-PHix process, stabilisation/solidification using cementitious binders and a range of thermal treatment processes are reviewed. Thermal treatment technologies convert APC residues combined with other wastes into inert glass or glass-ceramics that encapsulate heavy metals. The waste management industry will inevitably use the cheapest available option for treating APC residues and strict interpretation and enforcement of waste legislation is required if new, potentially more sustainable technologies are to become commercially viable.

Bone regeneration: molecular and cellular interactions with calcium phosphate ceramics

PubMed Central

Barrère, Florence; van Blitterswijk, Clemens A; de Groot, Klaas

2006-01-01

Calcium phosphate bioceramics are widely used in orthopedic and dental applications and porous scaffolds made of them are serious candidates in the field of bone tissue engineering. They have superior properties for the stimulation of bone formation and bone bonding, both related to the specific interactions of their surface with the extracellular fluids and cells, ie, ionic exchanges, superficial molecular rearrangement and cellular activity. PMID:17717972

Devitrification studies of wollastonite-tricalcium phosphate eutectic glass.

PubMed

Magallanes-Perdomo, M; Pena, P; De Aza, P N; Carrodeguas, R G; Rodríguez, M A; Turrillas, X; De Aza, S; De Aza, A H

2009-10-01

The present paper describes and discusses the devitrification and crystallization process of wollastonite-tricalcium phosphate (W-TCP) eutectic glass. This process was studied in situ from room temperature up to 1375 degrees C, by neutron diffractometry in vacuum. The data obtained were combined and compared with those performed in ambient atmosphere by differential thermal analysis and with those of samples fired in air at selected temperatures, and then cooled down and subsequently studied by laboratory XRD and field emission scanning electron microscopy fitted with energy X-ray dispersive spectroscopy. The experimental evidence indicates that the devitrification of W-TCP eutectic glass begins at approximately 870 degrees C with the crystallization of a Ca-deficient apatite phase, followed by wollastonite-2M (CaSiO(3)) crystallization at approximately 1006 degrees C. At 1375 degrees C, the bio-glass-ceramic is composed of quasi-rounded colonies formed by a homogeneous mixture of pseudowollastonite (CaSiO(3)) and alpha-tricalcium phosphate (Ca(3)(PO(4))(2)). This microstructure corresponds to irregular eutectic structures. It was also found that it is possible to obtain from the eutectic composition of the wollastonite-tricalcium phosphate binary system a wide range of bio-glass-ceramics, with different crystalline phases present, through appropriate design of thermal treatments.

Synthesis and mechanical behavior of β-tricalcium phosphate/titania composites addressed to regeneration of long bone segments.

PubMed

Sprio, Simone; Guicciardi, Stefano; Dapporto, Massimiliano; Melandri, Cesare; Tampieri, Anna

2013-01-01

Bioactive tricalcium phosphate/titania ceramic composites were synthesized by pressureless air sintering of mixed hydroxyapatite and titania (TiO2) powders. The sintering process was optimized to achieve dense ceramic bodies consisting in a bioactive/bioresorbable matrix (β-tricalcium phosphate) reinforced with defined amounts of sub-micron sized titania particles. Extensive chemico-physical and mechanical characterization was carried out on the resulting composites, which displayed values of flexural strength, fracture toughness and elastic modulus in the range or above the typical ranges of values manifested by human cortical bone. It was shown that titania particles provided a toughening effect to the calcium-phosphate matrix and a reinforcement in fracture strength, in comparison with sintered hydroxyapatite bodies characterized by similar relative density. The characteristics of the resulting composites, i.e. bioactivity/bioresorbability and ability of manifesting biomimetic mechanical behavior, are features that can promote processes of bone regeneration in load-bearing sites. Hence, in the perspective of developing porous bone scaffolds with high bioactivity and improved biomechanical behavior, TCP/TiO2 composites with controlled composition can be considered as very promising biomaterials for application in a field of orthopedics where no acceptable clinical solutions still exist. Copyright © 2012 Elsevier Ltd. All rights reserved.

Preparation and characterization of TiO2 and Si-doped octacalcium phosphate composite coatings on zirconia ceramics (Y-TZP) for dental implant applications

NASA Astrophysics Data System (ADS)

Bao, Lei; Liu, Jingxiao; Shi, Fei; Jiang, Yanyan; Liu, Guishan

2014-01-01

In order to prevent the low temperature degradation and improve the bioactivity of zirconia ceramic implants, TiO2 and Si-doped octacalcium phosphate composite coating was prepared on zirconia substrate. The preventive effect on low temperature degradation and surface morphology of the TiO2 layer were studied. Meanwhile, the structure and property changes of the bioactive coating after doping Si were discussed. The results indicate that the dense TiO2 layer, in spite of some microcracks, inhibited the direct contact of the water vapor with the sample's surface and thus prevented the low temperature degradation of zirconia substrates. The acceleration aging test shows that the ratio of the monoclinic phase transition decreased from 10% for the original zirconia substrate to 4% for the TiO2-coated substrate. As to the Si-doped octacalcium phosphate coating prepared by biomimetic method, the main phase composition of the coating was octacalcium phosphate. The morphology of the coating was lamellar-like, and the surface was uniform and continuous with no cracks being observed. It is suggested that Si was added into the coating both through substituting for PO43- and doping as NaSiO3.

Proceedings of the Asilomar Conference on Polymers (9th) Held on February 9-12, 1986 at Asilomar, California.

DTIC Science & Technology

1986-06-01

reticulated vitreous carbon material r ~ y n uniformity anc. material distribution. The material s * -p~s~Oro prismatic specimens. Four specimens had...with carbon fiber, hydroxylapatite ceramic (HA), tri-calcium phosphate ceramic (TCP), various organic acids, and calcium sulphate, we have been able to...filamentous carbon device coated with an absorbable polymer to prevent * premature fragmentation of the carbon fiber. Fracture repair has been effected

Method of waste stabilization via chemically bonded phosphate ceramics

DOEpatents

Wagh, Arun S.; Singh, Dileep; Jeong, Seung-Young

1998-01-01

A method for regulating the reaction temperature of a ceramic formulation process is provided comprising supplying a solution containing a monovalent alkali metal; mixing said solution with an oxide powder to create a binder; contacting said binder with bulk material to form a slurry; and allowing the slurry to cure. A highly crystalline waste form is also provided consisting of a binder containing potassium and waste substrate encapsulated by the binder.

Method of waste stabilization via chemically bonded phosphate ceramics

DOEpatents

Wagh, A.S.; Singh, D.; Jeong, S.Y.

1998-11-03

A method for regulating the reaction temperature of a ceramic formulation process is provided comprising supplying a solution containing a monovalent alkali metal; mixing said solution with an oxide powder to create a binder; contacting said binder with bulk material to form a slurry; and allowing the slurry to cure. A highly crystalline waste form is also provided consisting of a binder containing potassium and waste substrate encapsulated by the binder. 3 figs.

Radionuclide Retention Mechanisms in Secondary Waste-Form Testing: Phase II

DOE Office of Scientific and Technical Information (OSTI.GOV)

Um, Wooyong; Valenta, Michelle M.; Chung, Chul-Woo

2011-09-26

This report describes the results from laboratory tests performed at Pacific Northwest National Laboratory (PNNL) for Washington River Protection Solutions (WRPS) to evaluate candidate stabilization technologies that have the potential to successfully treat liquid secondary waste stream effluents produced by the Hanford Tank Waste Treatment and Immobilization Plant (WTP). WRPS is considering the design and construction of a Solidification Treatment Unit (STU) for the Effluent Treatment Facility (ETF) at Hanford. The ETF, a multi-waste, treatment-and-storage unit that has been permitted under the Resource Conservation and Recovery Act (RCRA), can accept dangerous, low-level, and mixed wastewaters for treatment. The STU needsmore » to be operational by 2018 to receive secondary liquid waste generated during operation of the WTP. The STU will provide the additional capacity needed for ETF to process the increased volume of secondary waste expected to be produced by WTP. This report on radionuclide retention mechanisms describes the testing and characterization results that improve understanding of radionuclide retention mechanisms, especially for pertechnetate, {sup 99}TcO{sub 4}{sup -} in four different waste forms: Cast Stone, DuraLith alkali aluminosilicate geopolymer, encapsulated fluidized bed steam reforming (FBSR) product, and Ceramicrete phosphate bonded ceramic. These data and results will be used to fill existing data gaps on the candidate technologies to support a decision-making process that will identify a subset of the candidate waste forms that are most promising and should undergo further performance testing.« less

Towards graphite-free hot zone for directional solidification of silicon

NASA Astrophysics Data System (ADS)

Dropka, Natasha; Buchovska, Iryna; Herrmann-Geppert, Iris; Klimm, Detlef; Kiessling, Frank M.; Degenhardt, Ulrich

2018-06-01

The reduction of SiC, Si3N4 and transition metals impurities in directionally solidified Si ingots poses one of the crucial challenges in the solar cells production. Particularly strong contamination comes from the graphite parts in the hot zone. Therefore, we selected three massive ceramic materials to replace graphite, developed the novel design of the crucible support and cover and compared the crystals grown in them with ingots from the standard graphite design. The experiments were performed for phosphorus n-doped silicon of G0 size. The ingots were compared with respect to O- and C-content, metal impurities, resistivity and lifetime. The superior performance of TiC relative to other ceramics was observed, particularly due to the lower concentration of substitutional carbon in Si ingot (up to 2.6 times) and the higher minority carrier lifetime of (up to 4.4 times) with narrow red zones.

Ceramic and non-ceramic hydroxyapatite as a bone graft material: a brief review.

PubMed

Dutta, S R; Passi, D; Singh, P; Bhuibhar, A

2015-03-01

Treatment of dental, craniofacial and orthopedic defects with bone graft substitutes has shown promising result achieving almost complete bone regeneration depending on product resorption similar to human bone's physicochemical and crystallographic characteristics. Among these, non-ceramic and ceramic hydroxyapatite being the main inorganic salt of bone is the most studied calcium phosphate material in clinical practices ever since 1970s and non-ceramic since 1985. Its "chemical similarity" with the mineralized phase of biologic bone makes it unique. Hydroxyapatite as an excellent carrier of osteoinductive growth factors and osteogenic cell populations is also useful as drug delivery vehicle regardless of its density. Porous ceramic and non-ceramic hydroxyapatite is osteoconductive, biocompatible and very inert. The need for bone graft material keeps on increasing with increased age of the population and the increased conditions of trauma. Recent advances in genetic engineering and doping techniques have made it possible to use non-ceramic hydroxyapatite in larger non-ceramic crystals and cluster forms as a successful bone graft substitute to treat various types of bone defects. In this paper we have mentioned some recently studied properties of hydroxyapatite and its various uses through a brief review of the literatures available to date.

Fifteen-year survival of anterior all-ceramic cantilever resin-bonded fixed dental prostheses.

PubMed

Kern, Matthias

2017-01-01

The aim of this follow-up study was to report the long-term outcome of all-ceramic cantilever resin-bonded fixed dental prostheses (RBFDPs). In 16 patients (mean age of 33.3±17.5years) 22 RBFDPs made from a glass-infiltrated alumina ceramic (In-Ceram) were inserted with a phosphate monomer containing luting agent after air-abrasion of the retainer wings. The abutment preparation included a shallow groove on the cingulum and a small proximal box. The restorations replacing 16 maxillary and 6 mandibular incisors were followed over a mean observation time of 188.7 months. No restoration debonded. Two RBFDPs fractured and were lost 48 and 214 months after insertion, respectively. The 10-year and 15-year survival rates were both 95.4% and dropped to 81.8% after 18 years. Anterior all-ceramic cantilever RBFDPs exhibited an excellent clinical longevity. Copyright © 2016 Elsevier Ltd. All rights reserved.

A New Biocompatible and Antibacterial Phosphate Free Glass-Ceramic for Medical Applications

NASA Astrophysics Data System (ADS)

Cabal, Belén; Alou, Luís; Cafini, Fabio; Couceiro, Ramiro; Sevillano, David; Esteban-Tejeda, Leticia; Guitián, Francisco; Torrecillas, Ramón; Moya, José S.

2014-06-01

In the attempt to find valid alternatives to classic antibiotics and in view of current limitations in the efficacy of antimicrobial-coated or loaded biomaterials, this work is focused on the development of a new glass-ceramic with antibacterial performance together with safe biocompatibility. This bactericidal glass-ceramic composed of combeite and nepheline crystals in a residual glassy matrix has been obtained using an antimicrobial soda-lime glass as a precursor. Its inhibitory effects on bacterial growth and biofilm formation were proved against five biofilm-producing reference strains. The biocompatibility tests by using mesenchymal stem cells derived from human bone indicate an excellent biocompatibility.

A New Biocompatible and Antibacterial Phosphate Free Glass-Ceramic for Medical Applications

PubMed Central

Cabal, Belén; Alou, Luís; Cafini, Fabio; Couceiro, Ramiro; Sevillano, David; Esteban-Tejeda, Leticia; Guitián, Francisco; Torrecillas, Ramón; Moya, José S.

2014-01-01

In the attempt to find valid alternatives to classic antibiotics and in view of current limitations in the efficacy of antimicrobial-coated or loaded biomaterials, this work is focused on the development of a new glass-ceramic with antibacterial performance together with safe biocompatibility. This bactericidal glass-ceramic composed of combeite and nepheline crystals in a residual glassy matrix has been obtained using an antimicrobial soda-lime glass as a precursor. Its inhibitory effects on bacterial growth and biofilm formation were proved against five biofilm-producing reference strains. The biocompatibility tests by using mesenchymal stem cells derived from human bone indicate an excellent biocompatibility. PMID:24961911

Field-assisted sintering and phase transition of ZnS-CaLa 2S 4 composite ceramics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Yiyu; Zhang, Lihua; Kisslinger, Kim

In the present study, zinc sulfide (ZnS) and calcium lanthanum sulfide (CaLa 2S 4, CLS) composite ceramics were consolidated via field-assisted sintering of 0.5ZnS-0.5CLS (volume ratio) composite powders at 800–1050 °C. Through sintering curve analyses and microstructural observations, it was determined that between 800 and 1000 °C, grain boundary diffusion was the main mechanism controlling grain growth for both the ZnS and CLS phases within the composite ceramics. The consolidated composite ceramics were determined to be composed of sphalerite ZnS, wurtzite ZnS and thorium phosphate CLS. The sphalerite-wurtzite phase transition of ZnS was further demonstrated to be accompanied by themore » formation of stacking faults and twins in the ceramics. Furthermore, it was also found that the addition of the CLS phase improved the indentation hardness of the ceramics relative to pure ZnS by homogeneous dispersion of ZnS and CLS small grains.« less

Field-assisted sintering and phase transition of ZnS-CaLa 2S 4 composite ceramics

DOE PAGES

Li, Yiyu; Zhang, Lihua; Kisslinger, Kim; ...

2017-07-17

In the present study, zinc sulfide (ZnS) and calcium lanthanum sulfide (CaLa 2S 4, CLS) composite ceramics were consolidated via field-assisted sintering of 0.5ZnS-0.5CLS (volume ratio) composite powders at 800–1050 °C. Through sintering curve analyses and microstructural observations, it was determined that between 800 and 1000 °C, grain boundary diffusion was the main mechanism controlling grain growth for both the ZnS and CLS phases within the composite ceramics. The consolidated composite ceramics were determined to be composed of sphalerite ZnS, wurtzite ZnS and thorium phosphate CLS. The sphalerite-wurtzite phase transition of ZnS was further demonstrated to be accompanied by themore » formation of stacking faults and twins in the ceramics. Furthermore, it was also found that the addition of the CLS phase improved the indentation hardness of the ceramics relative to pure ZnS by homogeneous dispersion of ZnS and CLS small grains.« less

Laser surface treatment for porous and textured Ca-P bio-ceramic coating on Ti-6Al-4V.

PubMed

Paital, Sameer R; Dahotre, Narendra B

2007-12-01

In the present paper the feasibility of depositing a porous calcium phosphate (CaP) bio-ceramic coating using a continuous wave Nd:YAG laser on a Ti-6Al-4V substrate has been demonstrated. The advantages offered by such porous bio-ceramic coating are its inertness combined with the mechanical stability of the highly convoluted interface that develops when bone grows into the pores of ceramic. The formation of different phases with varying laser fluences is studied using x-ray diffraction (XRD). A quantitative estimation of the crystallite size and relative amounts of Ti and other predominant phases such as TiO(2) and alpha-tricalcium phosphate (alpha-TCP) were obtained. An increase in the crystallite size with increasing laser fluence is observed for all the above three phases. It is observed that TiO(2) is the predominant phase for all laser fluences and there is an increase in the alpha-TCP phase with increasing laser fluence. Surface porosity measurements indicated a decreasing trend with increasing laser fluence. Microhardness measurements in the cross section of samples showed a maximum hardness within the coating. The bioactivity of the coatings was further demonstrated by the formation of an apatite-like layer on the surface of the sample after being immersed in a simulated biofluid.

Direct bioactive ceramics coating via reactive Growing Integration Layer method on α-Ti-alloy.

PubMed

Huang, Chi-Huang; Chen, Rong-Sheng; Yoshimura, Masahiro

2017-07-01

This paper demonstrates Ca-P-rich bio-ceramic and hydroxyapatite (HA) coatings formed directly from the solution of calcium acetate (CA) and sodium dihydrogen phosphate (SDP) on α-Ti-alloy substrates by Growing Integration Layer (GIL) technology under DC power supply. The composition of the α-Ti-alloy was Ti7Cu5Sn. The GIL coated films formed in 30min time with different voltages applied had porous and rough ceramic surfaces. They consisted mostly of various oxides like rutile, anatase, and calcium phosphates (including hydroxyapatite) that reduce corrosion rate and increase biocompatibility. An important feature was the reduction of Cu at the surfaces of the alloys. Furthermore, along with the applied voltage, the content of HA, the size of micro-pores, and hardness all increased, while the number of micro-pores in the ceramic membrane got reduced. The potential, current and resistance of corrosion were identified by potentiodynamic (PD) polarization and electrochemical impedance spectroscopy (EIS). The higher applied voltage improved the surface quality, HA formation rate, and the anti-corrosion behavior. Consequently, the samples - prepared at 350V and surface current density of 3A/cm 2 - possessed the most compact HA films, and also had the best corrosion resistance - in 0.9wt% NaCl solution at 37±1°C. Copyright © 2017. Published by Elsevier B.V.

Magnesium-phosphate-glass cements with ceramic-type properties

DOEpatents

Sugama, T.; Kukacka, L.E.

1982-09-23

Rapid setting magnesium phosphate (Mg glass) cementitious materials consisting of magnesium phosphate cement paste, polyborax and water-saturated aggregate, exhibits rapid setting and high early strength characteristics. The magnesium glass cement is prepared from a cation-leachable powder and a bivalent metallic ion-accepting liquid such as an aqueous solution of diammonium phosphate and ammonium polyphosphate. The cation-leachable powder includes a mixture of two different magnesium oxide powders processed and sized differently which when mixed with the bivalent metallic ion-accepting liquid provides the magnesium glass cement consisting primarily of magnesium ortho phosphate tetrahydrate, with magnesium hydroxide and magnesium ammonium phosphate hexahydrate also present. The polyborax serves as a set-retarder. The resulting magnesium mono- and polyphosphate cements are particularly suitable for use as a cementing matrix in rapid repair systems for deteriorated concrete structures as well as construction materials and surface coatings for fireproof structures.

Magnesium phosphate glass cements with ceramic-type properties

DOEpatents

Sugama, Toshifumi; Kukacka, Lawrence E.

1984-03-13

Rapid setting magnesium phosphate (Mg glass) cementitious materials consisting of magnesium phosphate cement paste, polyborax and water-saturated aggregate exhibiting rapid setting and high early strength characteristics. The magnesium glass cement is prepared from a cation-leachable powder and a bivalent metallic ion-accepting liquid such as an aqueous solution of diammonium phosphate and ammonium polyphosphate. The cation-leachable powder includes a mixture of two different magnesium oxide powders processed and sized differently which when mixed with the bivalent metallic ion-accepting liquid provides the magnesium glass cement consisting primarily of magnesium ortho phosphate tetrahydrate, with magnesium hydroxide and magnesium ammonium phosphate hexahydrate also present. The polyborax serves as a set-retarder. The resulting magnesium mono- and polyphosphate cements are particularly suitable for use as a cementing matrix in rapid repair systems for deteriorated concrete structures as well as construction materials and surface coatings for fireproof structures.

Surface degradation of glass ceramics after exposure to acidulated phosphate fluoride.

PubMed

Ccahuana, Vanessa Zulema S; Ozcan, Mutlu; Mesquita, Alfredo Mikail Melo; Nishioka, Renato Sussumo; Kimpara, Estevão Tomomitsu; Bottino, Marco Antonio

2010-01-01

This study evaluated the surface degradation effect of acidulated phosphate fluoride (APF) gel exposure on the glassy matrix ceramics as a function of time. Disc-shaped ceramic specimens (N = 120, 10/per ceramic material) were prepared in stainless steel molds (inner diameter: 5 mm, height: 2 mm) using 6 dental ceramics: 3 indicated for ceramic-fused-to-metal (Vita Omega 900, Carmen and Vita Titankeramik), 2 for all-ceramic (Vitadur Alpha and Finesse Low Fusing) and 1 for both types of restorations (IPS d.SIGN). The specimens were wet ground finished, ultrasonically cleaned and auto-glazed. All specimens were subjected to calculation of percentage of mass loss, surface roughness analysis and topographical description by scanning electron microscopy (SEM) before (0 min) and after exposure to 1.23 % APF gel for 4 min and 60 min representing short- and long-term etching effect, respectively. The data were analyzed using two-way ANOVA with repeated measures and Tukey's test (a=0.05). Significant effect of the type of the ceramics (p=0.0000, p=0.0031) and exposure time (p=0.0000) was observed in both surface roughness and percentage of mass loss values, respectively. The interaction factor between both parameters was also significant for both parameters (p=0.0904, p=0.0258). Both 4 min (0.44+/-0.1 - 0.81+/-0.2 microm) and 60 min (0.66+/-0.1 - 1.04+/-0.3 microm) APF gel exposure created significantly more surface roughness for all groups when compared to the control groups (0.33+/-0.2 - 0.68+/-0.2 microm) (p<0.05). There were no significant differences in percentage of mass loss between the ceramics at 4 min (p>0.05) but at 60 min exposure, IPS d.SIGN showed the highest percentage of mass loss (0.1151+/-0.11). The mean surface roughness for Vita Titankeramik (0.84+/-0.2 microm) and Finesse Low Fusing (0.74.+/-0.2 microm) was significantly higher than those of the other ceramics (0.59+/-0.1 microm - 0.49+/-0.1 microm) and Vita Titankeramik (p<0.05) regardless of the exposure time. A positive correlation was found between surface roughness and percentage of mass loss for all ceramic materials [(r=0.518 (Vitadur Alpha), r=0.405 (Vita Omega 900), r=0.580 (Carmen), r=0.687 (IPS d.SIGN), r=0.442 (Finesse Low Fusing), r=0.572 (Vita Titankeramik), Pearson's correlation coefficient)]. The qualitative SEM analysis showed evidence of corrosive attack on all of ceramics at varying degrees. The ceramics indicated for either metal-ceramic or all-ceramic restorations were all vulnerable to surface texture changes and mass loss after short-term and long-term APF gel exposure.

A new technique for cranioplasty with L-shaped titanium plates and combination ceramic implants composed of hydroxyapatite and tricalcium phosphate (Ceratite).

PubMed

Miyake, H; Ohta, T; Tanaka, H

2000-02-01

The use of hydroxyapatite-based ceramics for cranioplasties has recently increased in Japan, because of the good cosmetic outcomes, biocompatibility, strength, osteoconductive properties, and lack of risk of disease transmission associated with these materials. However, miniplate fixation has not been possible for ceramic implants. We describe a new technique for miniplate fixation of ceramic implants. Combination ceramic implants composed of hydroxyapatite and tricalcium phosphate (Ceratite; NGK Spark Plug Co., Aichi, Japan) were used for cranioplasties. A slot and a pair of holes were cut in each Ceratite implant, for use as a fixation unit. We have also developed a new L-shaped titanium plate (HOMS Engineering Inc., Nagano, Japan) that fits into the fixation unit. We first insert an L-shaped titanium plate through the slot from the back surface of the Ceratite implant. We then bend the plate outward at the front surface of the Ceratite implant and fix it to the cranium of the patient with titanium screws. The Ceratite implant is usually firmly fixed to the cranium of the patient with three L-shaped titanium plates. Using L-shaped titanium plates and Ceratite implants, we successfully performed cranioplasties for seven patients with cranial defects resulting from external decompression craniotomies. The Ceratite implant exactly fit the bone window for each patient. Surgical maneuvers were simple and easy for all patients, permitting shorter operating times. All Ceratite implants were firmly fixed, and no postoperative infections have occurred. Our new technique for cranioplasty is simple and allows rigid fixation of Ceratite implants.

Effect of heavy metals and water content on the strength of magnesium phosphate cements.

PubMed

Buj, Irene; Torras, Josep; Casellas, Daniel; Rovira, Miquel; de Pablo, Joan

2009-10-15

In this paper the mechanical properties of magnesium potassium phosphate cements used for the Stabilization/Solidification (S/S) of galvanic wastes were investigated. Surrogate wastes (metal nitrate dissolutions) were employed containing Cd, Cr(III), Cu, Ni, Pb or Zn at a concentration of 25 g dm(-3) and different water-to-solid (W/S) ratios (0.3, 0.4, 0.5 and 0.6 dm(3)kg(-1)) have been employed. Cements were prepared by mixing hard burned magnesia of about 70% purity with potassium dihydrogen phosphate. Compressive strength and tensile strength of specimens were determined. In addition the volume of permeable voids was measured. It was found that when comparing pastes that the volume of permeable voids increases and mechanical strength decreases with the increase of water-to-solid ratio (W/S). Nevertheless pastes with the same material proportions containing different metals show different mechanical strength values. The hydration products were analyzed by XRD. With the increase of water content not previously reported hydration compound was detected: bobierrite.

Calcium phosphate-based coatings on titanium and its alloys.

PubMed

Narayanan, R; Seshadri, S K; Kwon, T Y; Kim, K H

2008-04-01

Use of titanium as biomaterial is possible because of its very favorable biocompatibility with living tissue. Titanium implants having calcium phosphate coatings on their surface show good fixation to the bone. This review covers briefly the requirements of typical biomaterials and narrowly focuses on the works on titanium. Calcium phosphate ceramics for use in implants are introduced and various methods of producing calcium phosphate coating on titanium substrates are elaborated. Advantages and disadvantages of each type of coating from the view point of process simplicity, cost-effectiveness, stability of the coatings, coating integration with the bone, cell behavior, and so forth are highlighted. Taking into account all these factors, the efficient method(s) of producing these coatings are indicated finally.

Engineering and Development Support of General Decon Technology for the DARCOM Installation Restoration Program. Task 4. General Technology Literature Searches (II) Solidification Techniques for Lagoon Waters

DTIC Science & Technology

1980-12-01

40.8 Sodium 70.1 Zinc 0.01 37 The process includes the following steps (Pichat et al., 1979): - neutralization precipitation (silicates, borates...Compressive Strength of Polyester - Encapsulated Sodium Sulfate Waste Composite ....... .............. 64 9. Deep Chemical Mixer Mounted on a Barge...zinc, copper, lead, manganese and tin; sodium salts of arsenate, borate, phosphate, iodate, and sulfide; and sulfate salts. Sulfate salts form calcium

Phosphate glasses for radioactive, hazardous and mixed waste immobilization

DOEpatents

Cao, H.; Adams, J.W.; Kalb, P.D.

1998-11-24

Lead-free phosphate glass compositions are provided which can be used to immobilize low level and/or high level radioactive wastes in monolithic waste forms. The glass composition may also be used without waste contained therein. Lead-free phosphate glass compositions prepared at about 900 C include mixtures from about 1--6 mole % iron (III) oxide, from about 1--6 mole % aluminum oxide, from about 15--20 mole % sodium oxide or potassium oxide, and from about 30--60 mole % phosphate. The invention also provides phosphate, lead-free glass ceramic glass compositions which are prepared from about 400 C to about 450 C and which includes from about 3--6 mole % sodium oxide, from about 20--50 mole % tin oxide, from about 30--70 mole % phosphate, from about 3--6 mole % aluminum oxide, from about 3--8 mole % silicon oxide, from about 0.5--2 mole % iron (III) oxide and from about 3--6 mole % potassium oxide. Method of making lead-free phosphate glasses are also provided. 8 figs.

Impregnation of β-tricalcium phosphate robocast scaffolds by in situ polymerization.

PubMed

Martínez-Vázquez, Francisco J; Perera, Fidel H; van der Meulen, Inge; Heise, Andreas; Pajares, Antonia; Miranda, Pedro

2013-11-01

Ring-opening polymerization of ε-caprolactone (ε-CL) and L-lactide (LLA) was performed to impregnate β-tricalcium phosphate (β-TCP) scaffolds fabricated by robocasting. Concentrated colloidal inks prepared from β-TCP commercial powders were used to fabricate porous structures consisting of a 3D mesh of interpenetrating rods. ε-CL and LLA were in situ polymerized within the ceramic structure by using a lipase and stannous octanoate, respectively, as catalysts. The results show that both the macropores inside the ceramic mesh and the micropores within the ceramic rods are full of polymer in either case. The mechanical properties of scaffolds impregnated by in situ polymerization (ISP) are significantly increased over those of the bare structures, exhibiting similar values than those obtained by other, more aggressive, impregnation methods such as melt-immersion (MI). ISP using enzymatic catalysts requires a reduced processing temperature which could facilitate the incorporation of growth factors and other drugs into the polymer composition, thus enhancing the bioactivity of the composite scaffold. The implications of these results for the optimization of the mechanical and biological performance of scaffolds for bone tissue engineering applications are discussed. Copyright © 2013 Wiley Periodicals, Inc.

Phosphorus solubility in basaltic glass: Limitations for phosphorus immobilization in glass and glass-ceramics.

PubMed

Tarrago, M; Garcia-Valles, M; Martínez, S; Neuville, D R

2018-05-11

The composition of sewage sludge from urban wastewater treatment plants is simulated using P-doped basalts. Electron microscopy analyses show that the solubility of P in the basaltic melt is limited by the formation of a liquid-liquid immiscibility in the form of an aluminosilicate phase and a Ca-Mg-Fe-rich phosphate phase. The rheological behavior of these compositions is influenced by both phase separation and nanocrystallization. Upon a thermal treatment, the glasses will crystallize into a mixture of inosilicates and spinel-like phases at low P contents and into Ca-Mg-Fe phosphate at high P contents. Hardness measurements yield values between 5.41 and 7.66 GPa, inside the range of commercial glasses and glass-ceramics. Leaching affects mainly unstable Mg 2+ -PO 4 3- complexes. Copyright © 2018 Elsevier Ltd. All rights reserved.

The influence of different cementation modes on the fracture resistance of feldspathic ceramic crowns.

PubMed

Groten, M; Pröbster, L

1997-01-01

One hundred twenty pressed feldspathic ceramic crowns were luted to 20 steel dies using six different cementation modes. Fracture resistance was tested under an angle of 45 degrees and was determined as the maximal fracture load. Crowns were tested with luting agent only (groups A and C) and after etching with hydrofluoric acid, silanating, and the application of a bonding agent (groups B, D, E, and F). The resulting means were: phosphate cement 294.3 (A) and 282.2 (B); glass-ionomer cement 217.2 (C) and 255.4 (D); resin composite 382.2 (E) and 687.6 (F). Statistical analysis revealed significantly greater fracture resistance (P < .01) of resin luted crowns. Bonding to the die almost doubled the fracture resistance. Conditioning of the inner surfaces of the crowns did not improve the fracture resistance of crowns luted using zinc phosphate or glass-ionomer cements.

Bioresorbable Ca-phosphate-polymer/metal and Fe-Ag nanocomposites for macro-porous scaffolds with tunable degradation and drug release

NASA Astrophysics Data System (ADS)

Gotman, I.; Swain, S. K.; Sharipova, A.; Gutmanas, E. Y.

2016-11-01

Bioresorbable implants are increasingly gaining popularity as an attractive alternative to traditional permanent bone healing devices. The advantage of bioresorbable implantable devices is that they slowly degrade over time and disappear once their "mission" is accomplished. Thus, no foreign material is left behind that can cause adverse effects on the host, such as long term local or systemic immune response and stress-shielding related bone atrophy. Resorbable materials considered for surgical implant applications include degradable polymers, Ca phosphate ceramics (CaP) and corrodible metals. Degradable polymers, such as polycaprolactone and lactic acid are weak, lack osteoconductivity and degrade to acidic products that can cause late inflammation. Resorbable CaP ceramics (e.g., β-TCP) are attractive materials for bone regeneration bear close resemblance to the bone mineral, however they are intrinsically brittle and thus unsuitable for use in load-bearing sites. Moreover, introducing high porosity required to encourage better cellular ingrowth into bone regeneration scaffolds is detrimental to the mechanical strength of the material. In present work we review and discuss our results on development of strong bioresorbable Ca-phosphate-polymer/metal nanonocomposites and highly porous scaffolds from them. By introduction of nanoscale ductile polymer or metal phase into CaP ceramic an attempt was made to mimic structure of natural bone, where nanocrystallites of CaP ceramic are bonded by thin collagen layers. Recent results on development of high strength scaffolds from Fe-Ag nanocomposites are also reported. High energy milling of powders followed by cold sintering—high pressure consolidation at ambient temperature in combination with modified porogen leaching method was employed for processing. The developed nanocomposites and scaffolds exhibited high mechanical strength coupled with measurable ductility, gradual lost weight and strength during immersion in physiological media and high permeability falling in the range of trabecular bone. The proposed low-temperature processing approach allows for incorporation of drugs into the residual nanopores without damaging the biomolecule activity.

Calcium phosphate ceramics in drug delivery

NASA Astrophysics Data System (ADS)

Bose, Susmita; Tarafder, Solaiman; Edgington, Joe; Bandyopadhyay, Amit

2011-04-01

Calcium phosphate (CaP) particulates, cements and scaffolds have attracted significant interest as drug delivery vehicles. CaP systems, including both hydroxyapaptite and tricalcium phosphates, possess variable stoichiometry, functionality and dissolution properties which make them suitable for cellular delivery. Their chemical similarity to bone and thus biocompatibility, as well as variable surface charge density contribute to their controlled release properties. Among specific research areas, nanoparticle size, morphology, surface area due to porosity, and chemistry controlled release kinetics are the most active. This article discusses CaP systems in their particulate, cements, and scaffold forms for drug, protein, and growth factor delivery toward orthopedic and dental applications.

Optimization of culture conditions for osteogenically-induced mesenchymal stem cells in β-tricalcium phosphate ceramics with large interconnected channels.

PubMed

Bernhardt, Anne; Lode, Anja; Peters, Fabian; Gelinsky, Michael

2011-06-01

The aim of this study was to optimize culture conditions for human mesenchymal stem cells (hMSCs) in β-tricalcium phosphate ceramics with large interconnected channels. Fully interconnected macrochannels comprising pore diameters of 750 µm and 1400 µm were inserted into microporous β-tricalcium phosphate (β-TCP) scaffolds by milling. Human bone marrow-derived MSCs were seeded into the scaffolds and cultivated for up to 3 weeks in both static and perfusion culture in the presence of osteogenic supplements (dexamethasone, β-glycerophosphate, ascorbate). It was confirmed by scanning electron microscopic investigations and histological staining that the perfusion culture resulted in uniform distribution of cells inside the whole channel network, whereas the statically cultivated cells were primarily found at the surface of the ceramic samples. It was also determined that perfusion with standard medium containing 10% fetal calf serum (FCS) led to a strong increase (seven-fold) of cell numbers compared with static cultivation observed after 3 weeks. Perfusion with low-serum medium (2% FCS) resulted in moderate proliferation rates which were comparable to those achieved in static culture, although the specific alkaline phosphatase (ALP) activity increased by a factor of more than 3 compared to static cultivation. Gene expression analysis of the ALP gene also revealed higher levels of ALP mRNA in low-serum perfused samples compared to statically cultivated constructs. In contrast, gene expression of the late osteogenic marker bone sialoprotein II (BSPII) was decreased for perfused samples compared to statically cultivated samples. Copyright © 2010 John Wiley & Sons, Ltd.

Study on the injectability of a novel glucose modified magnesium potassium phosphate chemically bonded ceramic.

PubMed

Tan, Yongshan; Dong, Jinmei; Yu, Hongfa; Li, Ying; Wen, Jing; Wu, Chengyou

2017-10-01

A novel magnesium potassium phosphate chemically bonded ceramic (MKPCBC) was prepared as a byproduct of boron-containing magnesium oxide (B-MgO) after extracting Li 2 CO 3 from salt lakes. In this work, the influence of glucose on the properties of MKPCBC, such as the setting time, compressive strength and hydration heat, was investigated. In addition, we studied the effect of the magnesium-phosphate ratio (M/P) and liquid-solid ratio (L/S) on the injectability of MKPCBC. The pH change in glucose modified MKPCBC paste was also investigated. The phase composition and microstructure were studied in detail by using X-ray diffraction (XRD) and scanning electron microscopy-energy dispersive spectrometry (SEM-EDS). The results show that the optimal content of glucose is 6wt%. The optimum proportions of M/P and L/S for MKPCBC are 1.5 and 0.25, respectively. The properties of the novel MPCBC can meet the requirements of biomaterials. In addition, the retardation mechanism of glucose on MKPCBC and the hydration mechanism of novel MKPCBC were studied in detail through the continuous monitoring of the phase composition and microstructure. Copyright © 2017. Published by Elsevier B.V.

Calcium phosphate ceramic systems in growth factor and drug delivery for bone tissue engineering: A review

PubMed Central

Bose, Susmita; Tarafder, Solaiman

2012-01-01

Calcium phosphates (CaPs) are the most widely used bone substitutes in bone tissue engineering due to their compositional similarities to bone mineral and excellent biocompatibility. In recent years, CaPs, especially hydroxyapatite and tricalcium phosphate, have attracted significant interest in simultaneous use as bone substitute and drug delivery vehicle, adding a new dimension to their application. CaPs are more biocompatible than many other ceramic and inorganic nanoparticles. Their biocompatibility and variable stoichiometry, thus surface charge density, functionality, and dissolution properties, make them suitable for both drug and growth factor delivery. CaP matrices and scaffolds have been reported to act as delivery vehicles for growth factors and drugs in bone tissue engineering. Local drug delivery in musculoskeletal disorder treatments can address some of the critical issues more effectively and efficiently than the systemic delivery. CaPs are used as coatings on metallic implants, CaP cements, and custom designed scaffolds to treat musculoskeletal disorders. This review highlights some of the current drug and growth factor delivery approaches and critical issues using CaP particles, coatings, cements, and scaffolds towards orthopedic and dental applications. PMID:22127225

Lanthanide (Nd, Gd) compounds with garnet and monazite structures. Powders synthesis by "wet" chemistry to sintering ceramics by Spark Plasma Sintering

NASA Astrophysics Data System (ADS)

Potanina, Ekaterina; Golovkina, Ludmila; Orlova, Albina; Nokhrin, Aleksey; Boldin, Maksim; Sakharov, Nikita

2016-05-01

Complex oxide Y2.5Nd0.5Al5O12 with garnet structure and phosphates NdPO4 and GdPO4 with monazite structure were obtained by using precipitation methods. Ceramics Y2.5Nd0.5Al5O12 and NdPO4 were processed by Spark Plasma Sintering (SPS). Relative density more 98%, sintering time did not exceed 8 min, sintering temperature 1330-1390 °C. Leaching rates of elements from ceramics were 10-6-10-7 g/(cm2 d). The process of ceramics sintering has two-stage character: the first step of sintering-compaction process is related to the plastic flow of the material, the second step-to the process of grain boundary diffusion and grain growth.

Ceramic Adhesive for High Temperatures

NASA Technical Reports Server (NTRS)

Stevens, Everett G.

1987-01-01

Fused-silica/magnesium-phosphate adhesive resists high temperatures and vibrations. New adhesive unaffected by extreme temperatures and vibrations. Assuring direct bonding of gap filters to tile sidewalls, adhesive obviates expensive and time-consuming task of removal, treatment, and replacement of tiles.

Surface degradation of glass ceramics after exposure to acidulated phosphate fluoride

PubMed Central

CCAHUANA, Vanessa Zulema S.; ÖZCAN, Mutlu; MESQUITA, Alfredo Mikail Melo; NISHIOKA, Renato Sussumo; KIMPARA, Estevão Tomomitsu; BOTTINO, Marco Antonio

2010-01-01

Objective This study evaluated the surface degradation effect of acidulated phosphate fluoride (APF) gel exposure on the glassy matrix ceramics as a function of time. Material and methods Disc-shaped ceramic specimens (N = 120, 10/per ceramic material) were prepared in stainless steel molds (inner diameter: 5 mm, height: 2 mm) using 6 dental ceramics: 3 indicated for ceramic-fused-to-metal (Vita Omega 900, Carmen and Vita Titankeramik), 2 for all-ceramic (Vitadur Alpha and Finesse® Low Fusing) and 1 for both types of restorations (IPS d.SIGN). The specimens were wet ground finished, ultrasonically cleaned and auto-glazed. All specimens were subjected to calculation of percentage of mass loss, surface roughness analysis and topographical description by scanning electron microscopy (SEM) before (0 min) and after exposure to 1.23 % APF gel for 4 min and 60 min representing short- and long-term etching effect, respectively. The data were analyzed using two-way ANOVA with repeated measures and Tukey`s test (α=0.05). Results Significant effect of the type of the ceramics (p=0.0000, p=0.0031) and exposure time (p=0.0000) was observed in both surface roughness and percentage of mass loss values, respectively. The interaction factor between both parameters was also significant for both parameters (p=0.0904, p=0.0258). Both 4 min (0.44±0.1 - 0.81±0.2 µm) and 60 min (0.66±0.1 - 1.04±0.3 µm) APF gel exposure created significantly more surface roughness for all groups when compared to the control groups (0.33±0.2 - 0.68±0.2 µm) (p<0.05). There were no significant differences in percentage of mass loss between the ceramics at 4 min (p>0.05) but at 60 min exposure, IPS d.SIGN showed the highest percentage of mass loss (0.1151±0.11). The mean surface roughness for Vita Titankeramik (0.84±0.2 µm) and Finesse® Low Fusing (0.74.±0.2 µm) was significantly higher than those of the other ceramics (0.59±0.1 µm - 0.49±0.1 µm) and Vita Titankeramik (p<0.05) regardless of the exposure time. A positive correlation was found between surface roughness and percentage of mass loss for all ceramic materials [(r=0.518 (Vitadur Alpha), r=0.405 (Vita Omega 900), r=0.580 (Carmen), r=0.687 (IPS d.SIGN), r=0.442 (Finesse® Low Fusing), r=0.572 (Vita Titankeramik), Pearson`s correlation coefficient)]. The qualitative SEM analysis showed evidence of corrosive attack on all of ceramics at varying degrees. Conclusions The ceramics indicated for either metal-ceramic or all-ceramic restorations were all vulnerable to surface texture changes and mass loss after short-term and long-term APF gel exposure. PMID:20485927

Microwave Crystallization of Lithium Aluminum Germanium Phosphate Solid-State Electrolyte.

PubMed

Mahmoud, Morsi M; Cui, Yuantao; Rohde, Magnus; Ziebert, Carlos; Link, Guido; Seifert, Hans Juergen

2016-06-23

Lithium aluminum germanium phosphate (LAGP) glass-ceramics are considered as promising solid-state electrolytes for Li-ion batteries. LAGP glass was prepared via the regular conventional melt-quenching method. Thermal, chemical analyses and X-ray diffraction (XRD) were performed to characterize the prepared glass. The crystallization of the prepared LAGP glass was done using conventional heating and high frequency microwave (MW) processing. Thirty GHz microwave (MW) processing setup were used to convert the prepared LAGP glass into glass-ceramics and compared with the conventionally crystallized LAGP glass-ceramics that were heat-treated in an electric conventional furnace. The ionic conductivities of the LAGP samples obtained from the two different routes were measured using impedance spectroscopy. These samples were also characterized using XRD and scanning electron microscopy (SEM). Microwave processing was successfully used to crystallize LAGP glass into glass-ceramic without the aid of susceptors. The MW treated sample showed higher total, grains and grain boundary ionic conductivities values, lower activation energy and relatively larger-grained microstructure with less porosity compared to the corresponding conventionally treated sample at the same optimized heat-treatment conditions. The enhanced total, grains and grain boundary ionic conductivities values along with the reduced activation energy that were observed in the MW treated sample was considered as an experimental evidence for the existence of the microwave effect in LAGP crystallization process. MW processing is a promising candidate technology for the production of solid-state electrolytes for Li-ion battery.

Faster, Less Expensive Dies Using RSP Tooling

NASA Astrophysics Data System (ADS)

Knirsch, James R.

2007-08-01

RSP Tooling is an indirect spray form additive process that can produce production tooling for virtually any forming process and from virtually any metal. In the past 24 months a significant amount of research and development has been performed. This resulted in an increase in the basic metallurgical understanding of what transpires during the rapid solidification of the metal, significant improvements in the production machine up time, ceramic developments that have improved finish, process changes that have resulted in a shorter lead time for tool delivery, and the testing of many new alloys. RSP stands for Rapid Solidification Process and is the key to the superior metallurgical properties that result from the technology. Most metals that are sprayed in the process leave the machine with the same physical properties as the same metal normally achieves through heat treatment and in some cases the properties are superior. Many new applications are being pursued including INVAR tools for aerospace composite materials, and bimetallic tools made from tool steel and beryllium copper for die casting and plastic injection molding. Recent feasibility studies have been performed with tremendous success.

Method of processing "BPS" glass ceramic and seals made therewith

DOEpatents

Reed, Scott T.; Stone, Ronald G.; McCollister, Howard L.; Wengert, deceased, Paul R.

1998-01-01

A glass ceramic composition, a glass ceramic-to-metal seal, and more specifically a hermetic glass ceramic-to-metal seal prepared by subjecting a glass composition comprising, by weight percent, SiO.sub.2 (65-80%), LiO.sub.2 (8-16%), Al.sub.2 O.sub.3 (2-8%), K.sub.2 O (1-8%), P.sub.2 O.sub.5 (1-5%), B.sub.2 O.sub.3 (0.5-7%), and ZnO (0-5%) to the following processing steps: 1) heating the glass composition in a belt furnace to a temperature sufficient to melt the glass and crystallize lithium phosphate, 2) holding at a temperature and for a time sufficient to create cristobalite nuclei, 3) cooling at a controlled rate and to a temperature to cause crystallization of lithium silicates and growth of cristobalite, and 4) still further cooling in stages to ambient temperature. This process produces a glass ceramic whose high coefficient of thermal expansion (up to 200.times.10.sup.-7 in/in/.degree.C.) permits the fabrication of glass ceramic-to-metal seals, and particularly hermetic glass ceramic seals to nickel-based and stainless steel alloys and copper.

Method of processing ``BPS`` glass ceramic and seals made therewith

DOEpatents

Reed, S.T.; Stone, R.G.; McCollister, H.L.; Wengert, P.R.

1998-10-13

A glass ceramic composition, a glass ceramic-to-metal seal, and more specifically a hermetic glass ceramic-to-metal seal prepared by subjecting a glass composition comprising, by weight percent, SiO{sub 2} (65--80%), LiO{sub 2} (8--16%), Al{sub 2}O{sub 3} (2--8%), K{sub 2}O (1--8%), P{sub 2}O{sub 5} (1--5%), B{sub 2}O{sub 3} (0.5--7%), and ZnO (0--5%) to the following processing steps: (1) heating the glass composition in a belt furnace to a temperature sufficient to melt the glass and crystallize lithium phosphate, (2) holding at a temperature and for a time sufficient to create cristobalite nuclei, (3) cooling at a controlled rate and to a temperature to cause crystallization of lithium silicates and growth of cristobalite, and (4) still further cooling in stages to ambient temperature. This process produces a glass ceramic whose high coefficient of thermal expansion (up to 200{times}10{sup {minus}7} in/in/C) permits the fabrication of glass ceramic-to-metal seals, and particularly hermetic glass ceramic seals to nickel-based and stainless steel alloys and copper. 5 figs.

Fabrication, Properties and Applications of Dense Hydroxyapatite: A Review

PubMed Central

Prakasam, Mythili; Locs, Janis; Salma-Ancane, Kristine; Loca, Dagnija; Largeteau, Alain; Berzina-Cimdina, Liga

2015-01-01

In the last five decades, there have been vast advances in the field of biomaterials, including ceramics, glasses, glass-ceramics and metal alloys. Dense and porous ceramics have been widely used for various biomedical applications. Current applications of bioceramics include bone grafts, spinal fusion, bone repairs, bone fillers, maxillofacial reconstruction, etc. Amongst the various calcium phosphate compositions, hydroxyapatite, which has a composition similar to human bone, has attracted wide interest. Much emphasis is given to tissue engineering, both in porous and dense ceramic forms. The current review focusses on the various applications of dense hydroxyapatite and other dense biomaterials on the aspects of transparency and the mechanical and electrical behavior. Prospective future applications, established along the aforesaid applications of hydroxyapatite, appear to be promising regarding bone bonding, advanced medical treatment methods, improvement of the mechanical strength of artificial bone grafts and better in vitro/in vivo methodologies to afford more particular outcomes. PMID:26703750

Effect of surface condition on the formation of solid lubricating films at high temperatures

NASA Technical Reports Server (NTRS)

Hanyaloglu, Bengi; Graham, E. E.

1992-01-01

Solid films were produced on active metal or ceramic surfaces using lubricants (such as tricresyl phosphate) delivered as a vapor at high temperatures, and the lubricity of these deposits under different dynamic wear conditions was investigated. A method is described for chemically activating ceramic surfaces resulting in a surface that could promote the formation of lubricating polymeric derivative of TCP. Experiments were carried out to evaluate the wear characteristics of unlubricated cast iron and of Sialon ceramic at 25 and 280 C, and lubricated with a vapor of TCP at 280 C. It is shown that continuous vapor phase lubrication of chemically treated Sialon reduced its coefficient of friction from 0.7 to less than 0.1.

A novel biphasic calcium phosphate derived from fish otoliths

NASA Astrophysics Data System (ADS)

Montañez-Supelano, N. D.; Sandoval-Amador, A.; Estupiñan-Durán, H. A.; Y Peña-Ballesteros, D.

2017-12-01

Calcium phosphates are bioceramics that have been widely used as bone substitutes because they encourage the formation of bone on their surface and can improve the healing of the bone. Hydroxyapatite HA (calcium/phosphorus ratio of 1.67) and tricalcium phosphate TCP (calcium/phosphorus ratio of 1.50) are the most common calcium phosphates. Natural materials have begun to be tested to make HA or TCP such as shells of cardiidae (family of mollusks) and eggshells. The calcium phosphate obtained has a high ability to precipitate apatite. In this work, the mixed phase ceramic of beta-Tri-calcium phosphate / hydroxyapatite (β-TCP/HA) was synthesized by aqueous precipitation from fish otoliths, which are monomineralic species composed of aragonite. Otoliths of the specie Plagioscion squamosissimus, commonly called the river croaker, were used. Techniques such as DRX, Raman spectroscopy and SEM-EDS were used to characterize the raw material and the obtained material. X-ray diffraction analysis revealed the presence of two crystalline phases of calcium phosphates with 86.2% crystallinity. SEM micrographs showed agglomeration of particles with porous structure and submicron particle sizes.

Aluminum phosphate ceramics for waste storage

DOEpatents

Wagh, Arun; Maloney, Martin D

2014-06-03

The present disclosure describes solid waste forms and methods of processing waste. In one particular implementation, the invention provides a method of processing waste that may be particularly suitable for processing hazardous waste. In this method, a waste component is combined with an aluminum oxide and an acidic phosphate component in a slurry. A molar ratio of aluminum to phosphorus in the slurry is greater than one. Water in the slurry may be evaporated while mixing the slurry at a temperature of about 140-200.degree. C. The mixed slurry may be allowed to cure into a solid waste form. This solid waste form includes an anhydrous aluminum phosphate with at least a residual portion of the waste component bound therein.

A new in vivo screening model for posterior spinal bone formation: comparison of ten calcium phosphate ceramic material treatments.

PubMed

Wilson, Clayton E; Kruyt, Moyo C; de Bruijn, Joost D; van Blitterswijk, Clemens A; Oner, F Cumhur; Verbout, Abraham J; Dhert, Wouter J A

2006-01-01

This study presents a new screening model for evaluating the influence of multiple conditions on the initial process of bone formation in the posterior lumbar spine of a large animal. This model uses cages designed for placement on the decorticated transverse process of the goat lumbar spine. Five conduction channels per cage, each be defined by a different material treatment, are open to both the underlying bone and overlying soft tissue. The model was validated in ten adult Dutch milk goats, with each animal implanted with two cages containing a total of ten calcium phosphate material treatments according to a randomized complete block design. The ten calcium phosphate ceramic materials were created through a combination of material chemistry (BCP, TCP, HA), sintering temperature (low, medium, high), calcination and surface roughness treatments. To monitor the bone formation over time, fluorochrome markers were administered at 3, 5 and 7 weeks and the animals were sacrificed at 9 weeks after implantation. Bone formation in the conduction channels was investigated by histology and histomorphometry of non-decalcified sections using traditional light and epifluorescent microscopy. According to both observed and measured bone formation parameters, materials were ranked in order of increasing magnitude as follows: low sintering temperature BCP (rough and smooth) approximately medium sintering temperature BCP approximately = TCP > calcined low sintering temperature HA > non-calcined low sintering temperature HA > high sintering temperature BCP (rough and smooth) > high sintering temperature HA (calcined and non-calcined). These results agree closely with those obtained in previous studies of osteoconduction and bioactivity of ceramics thereby validating the screening model presented in this study.

Phase equilibrium and preparation, crystallization and viscous sintering of glass in the alumina-silica-lanthanum phosphate system

NASA Astrophysics Data System (ADS)

He, Feng

The phase equilibrium, viscosity of melt-quenched glasses, and processing of sol-gel glasses of the alumina-silica-lanthanum phosphate system were studied. These investigations were directed towards serving the objective of synthesizing nano-structured ceramic-matrix-composites via controlled crystallization of glass precursors. The thermal stability, phase equilibrium, and liquidus temperatures of the alumina- and mullite-lanthanum phosphate systems are determined. An iridium wire heater was constructed to anneal samples up to 2200°C. Phosphorus evaporation losses were significant at high temperatures, especially over 1800°C. The tentative phase diagrams of the two quasi-binary systems were presented. The viscosity of the melt-quenched mullite-lanthanum phosphate glasses was measured by three different methods, including viscous sintering of glass powder compacts, neck formation between two Frenkel glass beads, and thermal analysis of the glass transition. Improved methodologies were developed for applying the interpretative mathematical models to the results of the sintered powder and thermal analytical experiments. Good agreement was found between all three methods for both absolute values and temperature dependence. A sol-gel process was developed as a low temperature route to producing glasses. A unique, single phase mullite gel capable of low temperature (575°C) mullitization was made from tetraethoxysilane and aluminum isopropoxide at room temperature in three days. Low temperature crystallization was attributed to the avoidance of phase segregation during gel formation and annealing. This was greatly enhanced by a combination of low temperature preheating in the amorphous state, a high heating rate during crystallization and low water content. The Al2O3 content in mullite (61-68 mol%) depended on the highest annealing temperature. Two mullite-lanthanum phosphate gels were made based upon modifying the chemical procedures used for the homogeneous single phase and heterogeneous diphasic mullite gels from same starting chemicals. Amorphous powders were obtained after optimized calcinations. Their different crystallization routes and sintering behavior were investigated and correlated with the different homogeneities of precursor gels. Structurally stable open, porous ceramics (up to 80% porosity) were produced from the single-phase gel derived powder, where gases exsolved during calcination caused foaming coincident with sintering. Translucent, dense glass ceramic was made from the calcined diphasic gel by hot-pressing.

Visualising phase change in a brushite-based calcium phosphate ceramic

PubMed Central

Bannerman, A.; Williams, R. L.; Cox, S. C.; Grover, L. M.

2016-01-01

The resorption of brushite-based bone cements has been shown to be highly unpredictable, with strong dependence on a number of conditions. One of the major factors is phase transformation, with change to more stable phases such as hydroxyapatite affecting the rate of resorption. Despite its importance, the analysis of phase transformation has been largely undertaken using methods that only detect crystalline composition and give no information on the spatial distribution of the phases. In this study confocal Raman microscopy was used to map cross-sections of brushite cylinders aged in Phosphate Buffered Saline, Foetal Bovine Serum, Dulbecco’s – Minimum Essential Medium (with and without serum). Image maps showed the importance of ageing medium on the phase composition throughout the ceramic structure. When aged without serum, there was dissolution of the brushite phase concomitant to the deposition of octacalcium phosphate (OCP) around the periphery of the sample. The deposition of OCP was detectable within five days and reduced the rate of brushite dissolution from the material. The use of serum, even at a concentration of 10vol% prevented phase transformation. This paper demonstrates the value of confocal Raman microscopy in monitoring phase change in biocements; it also demonstrates the problems with assessing material degradation in non-serum containing media. PMID:27604149

Visualising phase change in a brushite-based calcium phosphate ceramic

NASA Astrophysics Data System (ADS)

Bannerman, A.; Williams, R. L.; Cox, S. C.; Grover, L. M.

2016-09-01

The resorption of brushite-based bone cements has been shown to be highly unpredictable, with strong dependence on a number of conditions. One of the major factors is phase transformation, with change to more stable phases such as hydroxyapatite affecting the rate of resorption. Despite its importance, the analysis of phase transformation has been largely undertaken using methods that only detect crystalline composition and give no information on the spatial distribution of the phases. In this study confocal Raman microscopy was used to map cross-sections of brushite cylinders aged in Phosphate Buffered Saline, Foetal Bovine Serum, Dulbecco’s - Minimum Essential Medium (with and without serum). Image maps showed the importance of ageing medium on the phase composition throughout the ceramic structure. When aged without serum, there was dissolution of the brushite phase concomitant to the deposition of octacalcium phosphate (OCP) around the periphery of the sample. The deposition of OCP was detectable within five days and reduced the rate of brushite dissolution from the material. The use of serum, even at a concentration of 10vol% prevented phase transformation. This paper demonstrates the value of confocal Raman microscopy in monitoring phase change in biocements; it also demonstrates the problems with assessing material degradation in non-serum containing media.

The thermal stability of hydroxyapatite in biphasic calcium phosphate ceramics.

PubMed

Nilen, R W N; Richter, P W

2008-04-01

Biphasic calcium phosphate ceramics (BCP) comprising a mix of non-resorbable hydroxyapatite (HA) and resorbable beta-tricalcium phosphate (beta-TCP) are particularly suitable materials for synthetic bone substitute applications. In this study, HA synthesised by solid state reaction was mechanically mixed with beta-TCP, then sintered to form a suite of BCP materials with a wide range of HA/beta-TCP phase content ratios. The influence of sintering temperature and composition on the HA thermal stability was quantified by X-ray diffraction (XRD). The pre-sinter beta-TCP content was found to strongly affect the post-sinter HA/beta-TCP ratio by promoting the thermal decomposition of HA to beta-TCP, even at sintering temperatures as low as 850 degrees C. For BCP material with pre-sinter HA/beta-TCP = 40/60 wt%, approximately 80% of the HA decomposed to beta-TCP during sintering at 1000 degrees C. Furthermore, the HA content appeared to influence the reverse transformation of alpha-TCP to beta-TCP expected upon gradual cooling from sintering temperatures greater than 1125 degrees C. Because the HA/beta-TCP ratio dominantly determines the rate and extent of BCP resorption in vivo, the possible thermal decomposition of HA during BCP synthesis must be considered, particularly if high temperature treatments are involved.

Femtosecond laser induced fixation of calcium alkali phosphate ceramics on titanium alloy bone implant material.

PubMed

Symietz, Christian; Lehmann, Erhard; Gildenhaar, Renate; Krüger, Jörg; Berger, Georg

2010-08-01

Femtosecond lasers provide a novel method of attaching bioceramic material to a titanium alloy, thereby improving the quality of bone implants. The ultrashort 30 fs laser pulses (790 nm wavelength) penetrate a thin dip-coated layer of fine ceramic powder, while simultaneously melting a surface layer of the underlying metal. The specific adjustment of the laser parameters (pulse energy and number of pulses per spot) avoids unnecessary melting of the bioactive calcium phosphate, and permits a defined thin surface melting of the metal, which in turn is not heated throughout, and therefore maintains its mechanical stability. It is essential to choose laser energy densities that correspond to the interval between the ablation fluences of both materials involved: about 0.1-0.4 Jcm(-2). In this work, we present the first results of this unusual technique, including laser ablation studies, scanning electron microscopy and optical microscope images, combined with EDX data. Copyright 2010 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

In vitro degradation and cell response of calcium carbonate composite ceramic in comparison with other synthetic bone substitute materials.

PubMed

He, Fupo; Zhang, Jing; Yang, Fanwen; Zhu, Jixiang; Tian, Xiumei; Chen, Xiaoming

2015-05-01

The robust calcium carbonate composite ceramics (CC/PG) can be acquired by fast sintering calcium carbonate at a low temperature (650 °C) using a biocompatible, degradable phosphate-based glass (PG) as sintering agent. In the present study, the in vitro degradation and cell response of CC/PG were assessed and compared with 4 synthetic bone substitute materials, calcium carbonate ceramic (CC), PG, hydroxyapatite (HA) and β-tricalcium phosphate (β-TCP) ceramics. The degradation rates in decreasing order were as follows: PG, CC, CC/PG, β-TCP, and HA. The proliferation of rat bone mesenchymal stem cells (rMSCs) cultured on the CC/PG was comparable with that on CC and PG, but inferior to HA and β-TCP. The alkaline phosphatase (ALP) activity of rMSCs on CC/PG was lower than PG, comparable with β-TCP, but higher than HA. The rMSCs on CC/PG and PG had enhanced gene expression in specific osteogenic markers, respectively. Compared to HA and β-TCP, the rMSCs on the CC/PG expressed relatively lower level of collagen I and runt-related transcription factor 2, but showed more considerable expression of osteopontin. Although CC, PG, HA, and β-TCP possessed impressive performances in some specific aspects, they faced extant intrinsic drawbacks in either degradation rate or mechanical strength. Based on considerable compressive strength, moderate degradation rate, good cell response, and being free of obvious shortcoming, the CC/PG is promising as another choice for bone substitute materials. Copyright © 2015 Elsevier B.V. All rights reserved.

Synthesization and characterization of poly(lactic-co-glycolic acid) / calcium phosphate bone cement from crab shells

NASA Astrophysics Data System (ADS)

Hanan, M. R. Abdul; Daud, N. M.; Ismail, L. H.; Saidin, S.

2017-05-01

An injectable calcium phosphate (CaP) bone cement has been widely used for musculoskeletal and bone disorder due to its biocompatible and osteoconductive properties. In this study, CaP was successfully synthesized from crab shells by a wet chemical route. Poly(lactic-co-glycolic acid) (PLGA) microspheres which have been produced through a double emulsion technique were incorporated into the CaP mixture for the purpose of bone cement solidification. The ratio of both compounds, CaP and PLGA, were set at 8:2. The CaP and PLGA/CaP bone cement were analyzed by ATR-FTIR, FESEM-EDX and contact angle analyses. The bone cement was composed of CaP and PLGA where the micro-powders of CaP were agglomerated on the PLGA microspheres. Addition of the PLGA has increased the hydrophilicity of the bone cement which will be beneficial for materials degradation and bone integration.

Observations on infiltration of silicon carbide compacts with an aluminium alloy

NASA Technical Reports Server (NTRS)

Asthana, R.; Rohatgi, P. K.

1992-01-01

The melt infiltration of ceramic particulates permits an opportunity to observe such fundamental materials phenomena as nucleation, dynamic wetting and growth in constrained environments. Experimental observations are presented on the infiltration behavior and matrix microstructures that form when porous compacts of platelet-shaped single crystals of alpha- (hexagonal) silicon carbide are infiltrated with a liquid 2014 Al alloy. The infiltration process involved counter gravity infiltration of suitably tamped and preheated compacts of silicon carbide platelets under an external pressure in a special pressure chamber for a set period, then by solidification of the infiltrant metal in the interstices of the bed at atmospheric pressure.

Bonding to oxide ceramics—laboratory testing versus clinical outcome.

PubMed

Kern, Matthias

2015-01-01

Despite a huge number of published laboratory bonding studies on dental oxide ceramics clinical long-term studies on resin bonded oxide ceramic restorations are rare. The purpose of this review is to present the best available clinical evidence for successful bonding of dental oxide ceramic restorations. Clinical trials with resin-bonded restorations that had no or only limited mechanical retention and were made from alumina or zirconia ceramic were identified using an electronic search in PubMed database. Overall 10 publications with clinical trials could be identified. Their clinical outcome was compared with that laboratory bond strength studies. Clinical data provide strong evidence that air-abrasion at a moderate pressure in combination with using phosphate monomer containing primers and/or luting resins provide long-term durable bonding to glass-infiltrated alumina and zirconia ceramic under the humid and stressful oral conditions. As simple and clinically reliable bonding methods to oxide ceramics exist, the rationale for development of alternative bonding methods might be reconsidered especially when these methods are more time consuming or require rather complicated and/or technique sensitive procedures. Copyright © 2014 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Characterization and spectroscopic studies of multi-component calcium zinc bismuth phosphate glass ceramics doped with iron ions

NASA Astrophysics Data System (ADS)

Kumar, A. Suneel; Narendrudu, T.; Suresh, S.; Ram, G. Chinna; Rao, M. V. Sambasiva; Tirupataiah, Ch.; Rao, D. Krishna

2018-04-01

Glass ceramics with the composition 10CaF2-20ZnO-(15-x)Bi2O3-55P2O5:x Fe2O3(0≤x≤2.5) were synthesized by melt-quenching technique and heat treatment. These glass ceramics were characterized by XRD and SEM. Spectroscopic studies such as optical absorption, EPR were also carried out on these glass ceramics. From the absorption spectra the observed bands around 438 and 660nm are the octahedral transitions of Fe3+ (d5) ions and another band at about 536 nm is the tetrahedral transition of Fe3+ (d5) ions. The absorption spectrum also consist of a band around 991 nm and is attributed to the octahedral transition of Fe2+ ions. The EPR spectra of the prepared glass ceramics have exhibited two resonance signals one at g1=4.32 and another signal at g2=2.008. The observed decrease in band gap energy up to 2 mol% Fe2O3 doped glass ceramics is an evidence for the change of environment around iron ions and ligands from more covalent to less covalent (ionic) and induces higher concentration of NBOs which causes the depolymerization of the glass ceramic network.

The structure and properties of boron carbide ceramics modified by high-current pulsed electron-beam

NASA Astrophysics Data System (ADS)

Ivanov, Yuri; Tolkachev, Oleg; Petyukevich, Maria; Teresov, Anton; Ivanova, Olga; Ikonnikova, Irina; Polisadova, Valentina

2016-01-01

The present work is devoted to numerical simulation of temperature fields and the analysis of structural and strength properties of the samples surface layer of boron carbide ceramics treated by the high-current pulsed electron-beam of the submillisecond duration. The samples made of sintered boron carbide ceramics are used in these investigations. The problem of calculating the temperature field is reduced to solving the thermal conductivity equation. The electron beam density ranges between 8…30 J/cm2, while the pulse durations are 100…200 μs in numerical modelling. The results of modelling the temperature field allowed ascertaining the threshold parameters of the electron beam, such as energy density and pulse duration. The electron beam irradiation is accompanied by the structural modification of the surface layer of boron carbide ceramics either in the single-phase (liquid or solid) or two-phase (solid-liquid) states. The sample surface of boron carbide ceramics is treated under the two-phase state (solid-liquid) conditions of the structural modification. The surface layer is modified by the high-current pulsed electron-beam produced by SOLO installation at the Institute of High Current Electronics of the Siberian Branch of the Russian Academy of Sciences, Tomsk, Russia. The elemental composition and the defect structure of the modified surface layer are analyzed by the optical instrument, scanning electron and transmission electron microscopes. Mechanical properties of the modified layer are determined measuring its hardness and crack resistance. Research results show that the melting and subsequent rapid solidification of the surface layer lead to such phenomena as fragmentation due to a crack network, grain size reduction, formation of the sub-grained structure due to mechanical twinning, and increase of hardness and crack resistance.

Processing highly porous calcium phosphate ceramics for use in bioreactor cores for culturing human liver cells in-vitro

NASA Astrophysics Data System (ADS)

Finoli, Anthony

Chronic liver disease is the 11th highest cause of death in the United States claiming over 30,000 lives in 2009. The current treatment for chronic liver failure is liver transplantation but the availability of tissue is far less than the number of patients in need. To develop human liver tissue in the lab a 3D culturing environment must be created to support the growth of a complex tissue. Hydroxyapatite (HAp) has been chosen as a scaffold material because of its biocompatibility in the body and the ability to create a bioresorbable scaffold. By using a ceramic material, it is possible to create a three dimensional, protective environment in which tissue can grow. The first part of this study is to examine the behavior of adult human liver cells grown on composites of HAp and different biocompatible hydrogels. Porous HAp has been created using an emulsion foaming technique and cells are injected into the structure after being suspended in a hydrogel and are kept in culture for up to 28 days. Functional assays, gene expression and fluorescent microscopy will be used to examine these cultures. The second part of this study will be to develop a processing technique to create a resorbable scaffold that incorporates a vascular system template. Previous experiments have shown the high temperature decomposition of HAp into resorbable calcium phosphates will be used to create a multiphase material. By controlling the amount of transformation product formed, it is proposed that the resorption of the scaffold can be tailored. To introduce a pore network to guide the growth of a vascular system, a positive-negative casting technique has also been developed. A positive polymer copy can be made of a natural vascular system and ceramic is foamed around the copy. During sintering, the polymer is pyrolyzed leaving a multiscale pore network in the ceramic. By combining these techniques, it is proposed that a calcium phosphate bioreactor core can be processed that is suitable for the culturing of human liver tissue.

Simultaneous stabilization/solidification of Mn2+ and NH4+-N from electrolytic manganese residue using MgO and different phosphate resource.

PubMed

Shu, Jiancheng; Wu, Haiping; Liu, Renlong; Liu, Zuohua; Li, Bing; Chen, Mengjun; Tao, Changyuan

2018-02-01

This study examined simultaneous stabilization and solidification (S/S) of Mn 2+ and NH 4 + -N from electrolytic manganese residue (EMR) using MgO and different phosphate resource. The characteristics of EMR NH 4 + -N and Mn 2+ S/S behavior, S/S mechanisms, leaching test and economic analysis, were investigated. The results show that the S/S efficiency of Mn 2+ and NH 4 + -N could reach 91.58% and 99.98%, respectively, and the pH value is 8.75 when the molar ratio of Mg:P is 3:1 and the dose of PM (MgO and Na 3 PO 4 ·12H 2 O) is 8wt%. In this process, Mn 2+ could mainly be stabilized in the forms of Mn(H 2 PO 4 ) 2 ·2H 2 O, Mn 3 (PO 4 ) 2 ·3H 2 O, Mn(OH) 2 , and MnOOH, and NH 4 + -N in the form of NH 4 MgPO 4 ·6H 2 O. Economic evaluation indicates that using PM process has a lower cost than HPM and HOM process for the S/S of Mn 2+ and NH 4 + -N from EMR at the same stabilization agent dose. Leaching test values of all the measured metals are within the permitted level for the GB8978-1996 test suggested when the dose of PM, HPM and HOM is 8wt%. Copyright © 2017 Elsevier Inc. All rights reserved.

Effects of single pulse energy on the properties of ceramic coating prepared by micro-arc oxidation on Ti alloy

NASA Astrophysics Data System (ADS)

Wang, Jun-Hua; Wang, Jin; Lu, Yan; Du, Mao-Hua; Han, Fu-Zhu

2015-01-01

The effects of single pulse energy on the properties of ceramic coating fabricated on a Ti-6Al-4V alloy via micro-arc oxidation (MAO) in aqueous solutions containing aluminate, phosphate, and some additives are investigated. The thickness, micro-hardness, surface and cross-sectional morphology, surface roughness, and compositions of the ceramic coating are studied using eddy current thickness meter, micro-hardness tester, JB-4C Precision Surface roughness meter, scanning electron microscopy (SEM) and X-ray diffraction (XRD). Single pulse energy remarkably influences the ceramic coating properties. The accumulative time of impulse width is an important parameter in the scientific and rational measurement of the film forming law of ceramic coating. The ceramic coating thickness approximately linearly increases with the cumulative time of impulse width. Larger impulse width resulted in higher single pulse energy, film forming rates and thicker ceramic coating thickness. The sizes of oxide particles, micro-pores and micro-cracks slightly increase with impulse width and single pulse energy. The main surface conversion products generated during MAO process in aqueous solutions containing aluminate are rutile TiO2, anatase TiO2, and a large amount of Al2TiO5. The effects of single pulse energy on the micro-hardness and phase composition of ceramic coating are not as evident as those of frequency and duty cycle.

Silk coating on a bioactive ceramic scaffold for bone regeneration: effective enhancement of mechanical and in vitro osteogenic properties towards load-bearing applications.

PubMed

Li, Jiao Jiao; Roohani-Esfahani, Seyed-Iman; Kim, Kyungsook; Kaplan, David L; Zreiqat, Hala

2017-06-01

Bioactive ceramic scaffolds represent competitive choices for clinical bone reconstruction, but their widespread use is restricted by inherent brittleness and weak mechanical performance under load. This study reports the development of strong and tough bioactive scaffolds suitable for use in load-bearing bone reconstruction. A strong and bioactive ceramic scaffold (strontium-hardystonite-gahnite) is combined with single and multiple coating layers of silk fibroin to enhance its toughness, producing composite scaffolds which match the mechanical properties of cancellous bone and show enhanced capacity to promote in vitro osteogenesis. Also reported for the first time is a comparison of the coating effects obtained when a polymeric material is coated on ceramic scaffolds with differing microstructures, namely the strontium-hardystonite-gahnite scaffold with high-density struts as opposed to a conventional ceramic scaffold, such as biphasic calcium phosphate, with low-density struts. The results show that silk coating on a unique ceramic scaffold can lead to simple and effective enhancement of its mechanical and biological properties to suit a wider range of applications in clinical bone reconstruction, and also establish the influence of ceramic microstructure on the effectiveness of silk coating as a method of reinforcement when applied to different types of ceramic bone graft substitutes. Copyright © 2015 John Wiley & Sons, Ltd. Copyright © 2015 John Wiley & Sons, Ltd.

Mussel-inspired bioceramics with self-assembled Ca-P/polydopamine composite nanolayer: preparation, formation mechanism, improved cellular bioactivity and osteogenic differentiation of bone marrow stromal cells.

PubMed

Wu, Chengtie; Han, Pingping; Liu, Xiaoguo; Xu, Mengchi; Tian, Tian; Chang, Jiang; Xiao, Yin

2014-01-01

The nanostructured surface of biomaterials plays an important role in improving their in vitro cellular bioactivity as well as stimulating in vivo tissue regeneration. Inspired by the mussel's adhesive versatility, which is thought to be due to the plaque-substrate interface being rich in 3,4-dihydroxy-l-phenylalamine (DOPA) and lysine amino acids, in this study we developed a self-assembly method to prepare a uniform calcium phosphate (Ca-P)/polydopamine composite nanolayer on the surface of β-tricalcium phosphate (β-TCP) bioceramics by soaking β-TCP bioceramics in Tris-dopamine solution. It was found that the addition of dopamine, reaction temperature and reaction time are three key factors inducing the formation of a uniform Ca-P/polydopamine composite nanolayer. The formation mechanism of a Ca-P/polydopamine composite nanolayer involved two important steps: (i) the addition of dopamine to Tris-HCl solution decreases the pH value and accelerates Ca and P ionic dissolution from the crystal boundaries of β-TCP ceramics; (ii) dopamine is polymerized to form self-assembled polydopamine film and, at the same time, nanosized Ca-P particles are mineralized with the assistance of polydopamine, in which the formation of polydopamine occurs simultaneously with Ca-P mineralization (formation of nanosized microparticles composed of calcium phosphate-based materials), and finally a self-assembled Ca-P/polydopamine composite nanolayer forms on the surface of the β-TCP ceramics. Furthermore, the formed self-assembled Ca-P/polydopamine composite nanolayer significantly enhances the surface roughness and hydrophilicity of β-TCP ceramics, and stimulates the attachment, proliferation, alkaline phosphate (ALP) activity and bone-related gene expression (ALP, OCN, COL1 and Runx2) of human bone marrow stromal cells. Our results suggest that the preparation of self-assembled Ca-P/polydopamine composite nanolayers is a viable method to modify the surface of biomaterials by significantly improving their surface physicochemical properties and cellular bioactivity for bone regeneration application. Copyright © 2013 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Phosphate glasses for radioactive, hazardous and mixed waste immobilization

DOEpatents

Cao, H.; Adams, J.W.; Kalb, P.D.

1999-03-09

Lead-free phosphate glass compositions are provided which can be used to immobilize low level and/or high level radioactive wastes in monolithic waste forms. The glass composition may also be used without waste contained therein. Lead-free phosphate glass compositions prepared at about 900 C include mixtures from about 1 mole % to about 6 mole % iron (III) oxide, from about 1 mole % to about 6 mole % aluminum oxide, from about 15 mole % to about 20 mole % sodium oxide or potassium oxide, and from about 30 mole % to about 60 mole % phosphate. The invention also provides phosphate, lead-free glass ceramic glass compositions which are prepared from about 400 C to about 450 C and which includes from about 3 mole % to about 6 mole % sodium oxide, from about 20 mole % to about 50 mole % tin oxide, from about 30 mole % to about 70 mole % phosphate, from about 3 mole % to about 6 mole % aluminum oxide, from about 3 mole % to about 8 mole % silicon oxide, from about 0.5 mole % to about 2 mole % iron (III) oxide and from about 3 mole % to about 6 mole % potassium oxide. Method of making lead-free phosphate glasses are also provided. 8 figs.

Phosphate glasses for radioactive, hazardous and mixed waste immobilization

DOEpatents

Cao, Hui; Adams, Jay W.; Kalb, Paul D.

1998-11-24

Lead-free phosphate glass compositions are provided which can be used to immobilize low level and/or high level radioactive wastes in monolithic waste forms. The glass composition may also be used without waste contained therein. Lead-free phosphate glass compositions prepared at about 900.degree. C. include mixtures from about 1 mole % to about 6 mole % iron (III) oxide, from about 1 mole % to about 6 mole % aluminum oxide, from about 15 mole % to about 20 mole % sodium oxide or potassium oxide, and from about 30 mole % to about 60 mole % phosphate. The invention also provides phosphate, lead-free glass ceramic glass compositions which are prepared from about 400.degree. C. to about 450.degree. C. and which includes from about 3 mole % to about 6 mole % sodium oxide, from about 20 mole % to about 50 mole % tin oxide, from about 30 mole % to about 70 mole % phosphate, from about 3 mole % to about 6 mole % aluminum oxide, from about 3 mole % to about 8 mole % silicon oxide, from about 0.5 mole % to about 2 mole % iron (III) oxide and from about 3 mole % to about 6 mole % potassium oxide. Method of making lead-free phosphate glasses are also provided.

Phosphate glasses for radioactive, hazardous and mixed waste immobilization

DOEpatents

Cao, Hui; Adams, Jay W.; Kalb, Paul D.

1999-03-09

Lead-free phosphate glass compositions are provided which can be used to immobilize low level and/or high level radioactive wastes in monolithic waste forms. The glass composition may also be used without waste contained therein. Lead-free phosphate glass compositions prepared at about 900.degree. C. include mixtures from about 1 mole % to about 6 mole %.iron (III) oxide, from about 1 mole % to about 6 mole % aluminum oxide, from about 15 mole % to about 20 mole % sodium oxide or potassium oxide, and from about 30 mole % to about 60 mole % phosphate. The invention also provides phosphate, lead-free glass ceramic glass compositions which are prepared from about 400.degree. C. to about 450.degree. C. and which includes from about 3 mole % to about 6 mole % sodium oxide, from about 20 mole % to about 50 mole % tin oxide, from about 30 mole % to about 70 mole % phosphate, from about 3 mole % to about 6 mole % aluminum oxide, from about 3 mole % to about 8 mole % silicon oxide, from about 0.5 mole % to about 2 mole % iron (III) oxide and from about 3 mole % to about 6 mole % potassium oxide. Method of making lead-free phosphate glasses are also provided.

[Mechanical properties of polylactic acid/beta-tricalcium phosphate composite scaffold with double channels based on three-dimensional printing technique].

PubMed

Lian, Qin; Zhuang, Pei; Li, Changhai; Jin, Zhongmin; Li, Dichen

2014-03-01

To improve the poor mechanical strength of porous ceramic scaffold, an integrated method based on three-dimensional (3-D) printing technique is developed to incorporate the controlled double-channel porous structure into the polylactic acid/beta-tricalcium phosphate (PLA/beta-TCP) reinforced composite scaffolds (double-channel composite scaffold) to improve their tissue regeneration capability and the mechanical properties. The designed double-channel structure inside the ceramic scaffold consisted of both primary and secondary micropipes, which parallel but un-connected. The set of primary channels was used for cell ingrowth, while the set of secondary channels was used for the PLA perfusion. Integration technology of 3-D printing technique and gel-casting was firstly used to fabricate the double-channel ceramic scaffolds. PLA/beta-TCP composite scaffolds were obtained by the polymer gravity perfusion process to pour PLA solution into the double-channel ceramic scaffolds through the secondary channel set. Microscope, porosity, and mechanical experiments for the standard samples were used to evaluate the composite properties. The ceramic scaffold with only the primary channel (single-channel scaffold) was also prepared as a control. Morphology observation results showed that there was no PLA inside the primary channels of the double-channel composite scaffolds but a dense interface layer between PLA and beta-TCP obviously formed on the inner wall of the secondary channels by the PLA penetration during the perfusion process. Finite element simulation found that the compressive strength of the double-channel composite scaffold was less than that of the single-channel scaffold; however, mechanical tests found that the maximum compressive strength of the double-channel composite scaffold [(21.25 +/- 1.15) MPa] was higher than that of the single-channel scaffold[ (9.76 +/- 0.64) MPa]. The double-channel composite scaffolds fabricated by 3-D printing technique have controlled complex micropipes and can significantly enhance mechanical properties, which is a promising strategy to solve the contradiction of strength and high-porosity of the ceramic scaffolds for the bone tissue engineering application.

Method for solidification of radioactive and other hazardous waste

DOEpatents

Anshits, Alexander G.; Vereshchagina, Tatiana A.; Voskresenskaya, Elena N.; Kostin, Eduard M.; Pavlov, Vyacheslav F.; Revenko, Yurii A.; Tretyakov, Alexander A.; Sharonova, Olga M.; Aloy, Albert S.; Sapozhnikova, Natalia V.; Knecht, Dieter A.; Tranter, Troy J.; Macheret, Yevgeny

2002-01-01

Solidification of liquid radioactive waste, and other hazardous wastes, is accomplished by the method of the invention by incorporating the waste into a porous glass crystalline molded block. The porous block is first loaded with the liquid waste and then dehydrated and exposed to thermal treatment at 50-1,000.degree. C. The porous glass crystalline molded block consists of glass crystalline hollow microspheres separated from fly ash (cenospheres), resulting from incineration of fossil plant coals. In a preferred embodiment, the porous glass crystalline blocks are formed from perforated cenospheres of grain size -400+50, wherein the selected cenospheres are consolidated into the porous molded block with a binder, such as liquid silicate glass. The porous blocks are then subjected to repeated cycles of saturating with liquid waste, and drying, and after the last cycle the blocks are subjected to calcination to transform the dried salts to more stable oxides. Radioactive liquid waste can be further stabilized in the porous blocks by coating the internal surface of the block with metal oxides prior to adding the liquid waste, and by coating the outside of the block with a low-melting glass or a ceramic after the waste is loaded into the block.

Space Station Furnace Facility. Volume 2: Summary of technical reports

NASA Technical Reports Server (NTRS)

1992-01-01

The Space Station Furnace Facility (SSFF) is a modular facility for materials research in the microgravity environment of the Space Station Freedom (SSF). The SSFF is designed for crystal growth and solidification research in the fields of electronic and photonic materials, metals and alloys, and glasses and ceramics, and will allow for experimental determination of the role of gravitational forces in the solidification process. The facility will provide a capability for basic scientific research and will evaluate the commercial viability of low-gravity processing of selected technologically important materials. In order to accommodate the furnace modules with the resources required to operate, SSFF developed a design that meets the needs of the wide range of furnaces that are planned for the SSFF. The system design is divided into subsystems which provide the functions of interfacing to the SSF services, conditioning and control for furnace module use, providing the controlled services to the furnace modules, and interfacing to and acquiring data from the furnace modules. The subsystems, described in detail, are as follows: Power Conditioning and Distribution Subsystem; Data Management Subsystem; Software; Gas Distribution Subsystem; Thermal Control Subsystem; and Mechanical Structures Subsystem.

Silver ion doped ceramic nano-powder coated nails prevent infection in open fractures: In vivo study.

PubMed

Kose, Nusret; Çaylak, Remzi; Pekşen, Ceren; Kiremitçi, Abdurrahman; Burukoglu, Dilek; Koparal, Savaş; Doğan, Aydın

2016-02-01

Despite improvement in operative techniques and antibiotic therapy, septic complications still occur in open fractures. We developed silver ion containing ceramic nano powder for implant coating to provide not only biocompatibility but also antibacterial activity to the orthopaedic implants. We hypothesised silver ion doped calcium phosphate based ceramic nano-powder coated titanium nails may prevents bacterial colonisation and infection in open fractures as compared with uncoated nails. 33 rabbits divided into three groups. In the first group uncoated, in the second group hydroxyapatite coated, and in the third group silver doped hydroxyapatite coated titanium nails were inserted left femurs of animals from knee regions with retrograde fashion. Before implantation of nails 50 μl solution containing 10(6)CFU/ml methicillin resistance Staphylococcus aureus (MRSA) injected intramedullary canal. Rabbits were monitored for 10 weeks. Blood was taken from rabbits before surgery and on 2nd, 6th and 10th weeks. Blood was analysed for biochemical parameters, blood count, C-reactive protein and silver levels. At the end of the 10 weeks animals were sacrificed and rods were extracted in a sterile fashion. Swab cultures were taken from intramedullary canal. Bacteria on titanium rods were counted. Liver, heart, spleen, kidney and central nervous tissues samples were taken for determining silver levels. Histopathological evaluation of bone surrounding implants was also performed. No significant difference was detected between the groups from hematologic, biochemical, and toxicological aspect. Microbiological results showed that less bacterial growth was detected with the use of silver doped ceramic coated implants compared to the other two groups (p=0.003). Accumulation of silver was not detected. No cellular inflammation was observed around the silver coated prostheses. No toxic effect of silver on bone cells was seen. Silver ion doped calcium phosphate based ceramic nano powder coating to orthopaedic implants may prevents bacterial colonisation and infection in open fractures compared with those for implants without any coating. Copyright © 2015 Elsevier Ltd. All rights reserved.

Effect of air-abrasion on the retention of zirconia ceramic crowns luted with different cements before and after artificial aging.

PubMed

Shahin, Ramez; Kern, Matthias

2010-09-01

The purpose of this in vitro study was to evaluate the effect of intaglio surface air-abrasion on the retention of CAD/CAM produced zirconia ceramic crowns cemented with three different types of cement. In addition the influence of artificial aging in masticatory simulator and thermocycling was tested. Extracted human premolars were prepared for all-ceramic crowns (12 degrees taper, 3 mm axial length). CAD/CAM zirconia crowns were manufactured. Half of the crowns were air-abraded with 50 microm alumina particles at 0.25 MPa, the rest was left as machined. The crowns were luted with zinc phosphate cement (Hoffmann), glass ionomer cement (Ketac Cem), or composite resin (Panavia 21), subgroups were either stored for 3 days in 37 degrees water bath or stored for 150 days in 37 degrees water bath, with additional 37,500 thermal cycles (5-55 degrees) and 300,000 cycles dynamic loading with 5 kg in a masticatory simulator. Then crown retention was measured in tension at a crosshead speed of 2 mm/min using a universal testing machine. Statistical analysis was performed with three-way ANOVA. Mean retention values were ranged from 2.8 to 7.1 MPa after 3 days and from 1.6 to 6.1 MPa after artificial aging. Air-abrasion significantly increased crown retention (p<0.001), while artificial aging decreased retention (p=0.017). In addition, the luting material had a significant influence on retention (p<0.001) with the adhesive luting resin providing the highest retention. The use of phosphate monomer containing composite resin on air-abraded zirconia ceramic can be recommended as most retentive luting method. Copyright 2010 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Long-term conversion of 45S5 bioactive glass-ceramic microspheres in aqueous phosphate solution.

PubMed

Fu, Hailuo; Rahaman, Mohamed N; Day, Delbert E; Huang, Wenhai

2012-05-01

The conversion of 45S5 glass and glass-ceramics to a hydroxyapatite (HA)-like material in vitro has been studied extensively, but only for short reaction times (typically <3 months). In this paper, we report for the first time on the long-term conversion of 45S5 glass-ceramic microspheres (designated 45S5c) in an aqueous phosphate solution. Microspheres of 45S5c (75-150 μm) were immersed for 10 years at room temperature (~25 °C) in K(2)HPO(4) solution with a concentration of 0.01 M or 1.0 M, and with a starting pH of 7.0 or 9.5. The reacted 45S5c microspheres and solutions were analyzed using structural and analytical techniques. Only 25-45 vol% of the 45S5c microspheres were converted to an HA-like material after the 10 year reaction. In solutions with a starting pH of 9.5, an increase in the K(2)HPO(4) concentration from 0.01 to 1.0 M resulted in a doubling of the volume of the microspheres converted to an HA-like material but had little effect on the composition of the HA-like product. In comparison, reaction of the 45S5c microspheres in the solution with a starting pH of 7.0 resulted in an HA-like product in the 0.01 M K(2)HPO(4) solution but a calcium pyrophosphate product, Ca(10)K(4)(P(2)O(7))(6).9H(2)O, in the 1.0 M solution. The consequences of these results for the long-term use of 45S5 glass-ceramics in biomedical applications are discussed.

[Quantitative determination of glass content in monazite glass-ceramics by IR technique].

PubMed

He, Yong; Zhang, Bao-min

2003-04-01

Monazite glass-ceramics consist of both monazite and metaphoshate glass phases. The absorption bands of both phases do not overlap each other, and the absorption intensities of bands 1,275 and 616 cm-1 vary with the glass contents. The correlation coefficient between logarithmic absorbance ratio of the two bands and glass contents was r = 0.9975 and its regression equation was y = 48.356 + 25.93x. The absorbance ratio of bands 952 and 616 cm-1 also varied with different ratios of Ce2O3/La2O3 in synthetic monazites, with r = 0.9917 and a regression equation y = 0.2211 exp (0.0221x). High correlation coefficients show that the IR technique could find new application in the quantitative analysis of glass content in phosphate glass-ceramics.

Mechanical stability of Ti6Al4V implant material after femtosecond laser irradiation

NASA Astrophysics Data System (ADS)

Symietz, Christian; Lehmann, Erhard; Gildenhaar, Renate; Hackbarth, Andreas; Berger, Georg; Krüger, Jörg

2012-07-01

The surface of a titanium alloy (Ti6Al4V) implant material was covered with a bioactive calcium alkali phosphate ceramic with the aim to accelerate the healing and to form a stronger bond to living bone tissue. To fix the ceramic powder we used a femtosecond laser, which causes a thin surface melting of the metal. It is a requirement to prove that the laser irradiation would not reduce the lifetime of implants. Here we present the results of mechanical stability tests, determined by the rotating bending fatigue strength of sample rods. After describing the sample surfaces and their modifications caused by the laser treatment we give evidence for an unchanged mechanical stability. This applies not only to the ceramic fixation but also to a comparatively strong laser ablation.

Study on different characteristics of doped tri calcium phosphate at different sintering temperatures

DOE Office of Scientific and Technical Information (OSTI.GOV)

Samanta, Sujan Krishna, E-mail: itssujan@rediffmail.com; Chanda, Abhijit, E-mail: abhijitchanda.biomed@gmail.com

2016-04-13

Pure β-tricalcium phosphate (β-TCP), Zn-doped (3wt %) β-TCP and Mg- doped (3wt %) β-TCP samples were prepared by using a wet chemical precipitation synthesis technique, followed by calcination at 800 °C in air. The developed materials were subjected to sintering at different temperatures. Density and porosity were compared. The X-ray diffractometry (XRD) and Fourier-transformed infrared (FTIR) spectrometer were used to examine the changes in crystalline phases and presence of functional groups of TCP ceramics. The scanning electron microscopy (SEM) was used to study the pore formation, pore size, grain size.

Stabilization/solidification of radioactive salt waste by using xSiO2-yAl2O3-zP2O5 (SAP) material at molten salt state.

PubMed

Park, Hwan-Seo; Kim, In-Tae; Cho, Yong-Zun; Eun, Hee-Chul; Lee, Han-Soo

2008-12-15

The molten salt waste from the pyroprocess is one of the problematic wastes to directly apply a conventional process such as vitrification or ceramization. This study suggested a novel method using a reactive material for metal chlorides at a molten temperature of salt waste, and then converting them into manageable product at a high temperature. The inorganic composite, SAP (SiO2-Al2O3-P2O5), synthesized by a conventional sol-gel process has three or four distinctive domains that are bonded sequentially, Si-O-Si-O-A-O-P-O-P. The P-rich phase in the SAP composite is unstable for producing a series of reactive sites when in contact with a molten LiCl salt. After the reaction, metal aluminosilicate, metal aluminophosphate, metal phosphates and gaseous chlorines are generated. From this process, the volatile salt waste is stabilized and it is possible to apply a high temperature process. The reaction products were fabricated successfully by using a borosilicate glass with an arbitrary composition as a chemical binder. There was a low possibility for the valorization of radionuclides up to 1200 degrees C, based on the result of the thermo gravimetric analysis. The Cs and Sr leach rates by the PCT-A method were about 1 x 10(-3) g/(m2 day). For the final disposal of the problematic salt waste, this approach suggested the design concept of an effective stabilizer for metal chlorides and revealed the chemical route to the fabrication of monolithic wasteform by using a composite as an example. Using this method, we could obtain a higher disposal efficiency and lower waste volume, compared with the present immobilization methods.

Materials for advanced rocket engine turbopump turbine blades

NASA Technical Reports Server (NTRS)

Chandler, W. T.

1985-01-01

A study program was conducted to identify those materials that will provide the greatest benefits as turbine blades for advanced liquid propellant rocket engine turbines and to prepare technology plans for the development of those materials for use in the 1990 through 1995 period. The candidate materials were selected from six classes of materials: single-crystal (SC) superalloys, oxide dispersion-strengthened (ODS) superalloys, rapid solidification processed (RSP) superalloys, directionally solidified eutectic (DSE) superalloys, fiber-reinforced superalloy (FRS) composites, and ceramics. Properties of materials from the six classes were compiled and evaluated and property improvements were projected approximately 5 years into the future for advanced versions of materials in each of the six classes.

[Clinical use of beta-tricalcium phosphate ceramics with patient's own bone in maxillary elevation with osteotome].

PubMed

Chen, Lu; Zhou, Wen-qing; Wu, Yan-ping; Lu, Jing-hua

2011-06-01

To evaluate the clinical value of using the patient's autogenous bone mixed with beta-tricalcium phosphate ceramics(β-TCP) for maxillary sinus lift with simultaneous implantation. Patients with loss of posterior teeth and bone height of maxillary sinus floor between 4-10mm underwent internal sinus floor elevation, the proportion of bone to β-TCP was 1:1 and the mixture was inserted into the sinus floor. All cases had simultaneously placed ITI implants.The final crown fabrication was taken 4-6 months after implanting. Twenty-one implants were inserted in 16 cases, the mean increase height was 4.2mm(2-6mm). There was clinical complaint of maxillary sinus inflammation in 1 case within 2 weeks, but the symptoms disappeared after antibiotic therapy. The remaining of 20 implants had no obvious complications. All implants had loaded for 32 months and were stable and well osseointegration on X-ray film. Maxillary sinus elevation with simultaneous implantation is an easy procedure. Implants can be stable for a long time.

Freckle Defect Formation near the Casting Interfaces of Directionally Solidified Superalloys

PubMed Central

Hong, Jianping; Ma, Dexin; Wang, Jun; Wang, Fu; Sun, Baode; Dong, Anping; Li, Fei; Bührig-Polaczek, Andreas

2016-01-01

Freckle defects usually appear on the surface of castings and industrial ingots during the directional solidification process and most of them are located near the interface between the shell mold and superalloys. Ceramic cores create more interfaces in the directionally solidified (DS) and single crystal (SX) hollow turbine blades. In order to investigate the location of freckle occurrence in superalloys, superalloy CM247 LC was directionally solidified in an industrial-sized Bridgman furnace. Instead of ceramic cores, Alumina tubes were used inside of the casting specimens. It was found that freckles occur not only on the casting external surfaces, but also appear near the internal interfaces between the ceramic core and superalloys. Meanwhile, the size, initial position, and area of freckle were investigated in various diameters of the specimens. The initial position of the freckle chain reduces when the diameter of the rods increase. Freckle area follows a linear relationship in various diameters and the average freckle fraction is 1.1% of cross sectional area of casting specimens. The flow of liquid metal near the interfaces was stronger than that in the interdendritic region in the mushy zone, and explained why freckle tends to occur on the outer or inner surfaces of castings. This new phenomenon suggests that freckles are more likely to occur on the outer or inner surfaces of the hollow turbine blades. PMID:28774050

Freckle Defect Formation near the Casting Interfaces of Directionally Solidified Superalloys.

PubMed

Hong, Jianping; Ma, Dexin; Wang, Jun; Wang, Fu; Sun, Baode; Dong, Anping; Li, Fei; Bührig-Polaczek, Andreas

2016-11-16

Freckle defects usually appear on the surface of castings and industrial ingots during the directional solidification process and most of them are located near the interface between the shell mold and superalloys. Ceramic cores create more interfaces in the directionally solidified (DS) and single crystal (SX) hollow turbine blades. In order to investigate the location of freckle occurrence in superalloys, superalloy CM247 LC was directionally solidified in an industrial-sized Bridgman furnace. Instead of ceramic cores, Alumina tubes were used inside of the casting specimens. It was found that freckles occur not only on the casting external surfaces, but also appear near the internal interfaces between the ceramic core and superalloys. Meanwhile, the size, initial position, and area of freckle were investigated in various diameters of the specimens. The initial position of the freckle chain reduces when the diameter of the rods increase. Freckle area follows a linear relationship in various diameters and the average freckle fraction is 1.1% of cross sectional area of casting specimens. The flow of liquid metal near the interfaces was stronger than that in the interdendritic region in the mushy zone, and explained why freckle tends to occur on the outer or inner surfaces of castings. This new phenomenon suggests that freckles are more likely to occur on the outer or inner surfaces of the hollow turbine blades.

Porous biomorphic silicon carbide ceramics coated with hydroxyapatite as prospective materials for bone implants.

PubMed

Gryshkov, Oleksandr; Klyui, Nickolai I; Temchenko, Volodymyr P; Kyselov, Vitalii S; Chatterjee, Anamika; Belyaev, Alexander E; Lauterboeck, Lothar; Iarmolenko, Dmytro; Glasmacher, Birgit

2016-11-01

Porous and cytocompatible silicon carbide (SiC) ceramics derived from wood precursors and coated with bioactive hydroxyapatite (HA) and HA-zirconium dioxide (HA/ZrO2) composite are materials with promising application in engineering of bone implants due to their excellent mechanical and structural properties. Biomorphic SiC ceramics have been synthesized from wood (Hornbeam, Sapele, Tilia and Pear) using a forced impregnation method. The SiC ceramics have been coated with bioactive HA and HA/ZrO2 using effective gas detonation deposition approach (GDD). The surface morphology and cytotoxicity of SiC ceramics as well as phase composition and crystallinity of deposited coatings were analyzed. It has been shown that the porosity and pore size of SiC ceramics depend on initial wood source. The XRD and FTIR studies revealed the preservation of crystal structure and phase composition of in the HA coating, while addition of ZrO2 to the initial HA powder resulted in significant decomposition of the final HA/ZrO2 coating and formation of other calcium phosphate phases. In turn, NIH 3T3 cells cultured in medium exposed to coated and uncoated SiC ceramics showed high re-cultivation efficiency as well as metabolic activity. The recultivation efficiency of cells was the highest for HA-coated ceramics, whereas HA/ZrO2 coating improved the recultivation efficiency of cells as compared to uncoated SiC ceramics. The GDD method allowed generating homogeneous HA coatings with no change in calcium to phosphorus ratio. In summary, porous and cytocompatible bio-SiC ceramics with bioactive coatings show a great promise in construction of light, robust, inexpensive and patient-specific bone implants for clinical application. Copyright © 2016 Elsevier B.V. All rights reserved.

Novel Method for Loading Microporous Ceramics Bone Grafts by Using a Directional Flow

PubMed Central

Seidenstuecker, Michael; Kissling, Steffen; Ruehe, Juergen; Suedkamp, Norbert P.; Mayr, Hermann O.; Bernstein, Anke

2015-01-01

The aim of this study was the development of a process for filling the pores of a β-tricalcium phosphate ceramic with interconnected porosity with an alginate hydrogel. For filling of the ceramics, solutions of alginate hydrogel precursors with suitable viscosity were chosen as determined by rheometry. For loading of the porous ceramics with the gel the samples were placed at the flow chamber and sealed with silicone seals. By using a vacuum induced directional flow, the samples were loaded with alginate solutions. The loading success was controlled by ESEM and fluorescence imaging using a fluorescent dye (FITC) for staining of the gel. After loading of the pores, the alginate is transformed into a hydrogel through crosslinking with CaCl2 solution. The biocompatibility of the obtained composite material was tested with a live dead cell staining by using MG-63 Cells. The loading procedure via vacuum assisted directional flow allowed complete filling of the pores of the ceramics within a few minutes (10 ± 3 min) while loading through simple immersion into the polymer solution or through a conventional vacuum method only gave incomplete filling. PMID:26703749

Doped Calcium Silicate Ceramics: A New Class of Candidates for Synthetic Bone Substitutes

PubMed Central

No, Young Jung; Li, Jiao Jiao; Zreiqat, Hala

2017-01-01

Doped calcium silicate ceramics (DCSCs) have recently gained immense interest as a new class of candidates for the treatment of bone defects. Although calcium phosphates and bioactive glasses have remained the mainstream of ceramic bone substitutes, their clinical use is limited by suboptimal mechanical properties. DCSCs are a class of calcium silicate ceramics which are developed through the ionic substitution of calcium ions, the incorporation of metal oxides into the base binary xCaO–ySiO2 system, or a combination of both. Due to their unique compositions and ability to release bioactive ions, DCSCs exhibit enhanced mechanical and biological properties. Such characteristics offer significant advantages over existing ceramic bone substitutes, and underline the future potential of adopting DCSCs for clinical use in bone reconstruction to produce improved outcomes. This review will discuss the effects of different dopant elements and oxides on the characteristics of DCSCs for applications in bone repair, including mechanical properties, degradation and ion release characteristics, radiopacity, and biological activity (in vitro and in vivo). Recent advances in the development of DCSCs for broader clinical applications will also be discussed, including DCSC composites, coated DCSC scaffolds and DCSC-coated metal implants. PMID:28772513

Optimization of calcium phosphate fine ceramic powders preparation

NASA Astrophysics Data System (ADS)

Sezanova, K.; Tepavitcharova, S.; Rabadjieva, D.; Gergulova, R.; Ilieva, R.

2013-12-01

The effect of biomimetic synthesis method, reaction medium and further precursor treatments on the chemical and phase composition, crystal size and morphology of calcium phosphates was examined. Nanosized calcium phosphate precursors were biomimetically precipitated by the method of continuous precipitation in three types of reaction media at pH 8: (i) SBF as an inorganic electrolyte system; (ii) organic (glycerine) modified SBF (volume ratio of 1:1); (iii) polymer (10 g/l xanthan gum or 10 g/l guar gum) modified SBF (volume ratio of 1:1). After maturation (24 h) the samples were lyophilized, calcinated at 300°C for 3 hours, and washed with water, followed by new gelation, lyophilization and step-wise (200, 400, 600, 800, and 1000°C, each for 3 hours) sintering. The reaction medium influenced the chemical composition and particle size but not the morphology of the calcium phosphate powders. In all studied cases bi-phase calcium phosphate fine powders with well-shaped spherical grains, consisting of β-tricalcium phosphate (β-TCP) and hydroxyapatite (HA) with a Ca/P ratio of 1.3 - 1.6 were obtained. The SBF modifiers decreased the particle size of the product in the sequence guar gum ˜ xanthan gum < glycerin < SBF medium.

Towards Synthesis and Usage of Actinide-Bearing REE Phosphate age Standards: A Progress Report

NASA Astrophysics Data System (ADS)

Pyle, J. M.; Cherniak, D. J.

2006-05-01

Electron microprobe (EMP) dates result from a concentration-time unit conversion, so use of a concentration- based (rather than isotope-ratio based) fictive age standard is warranted. This observation has motivated our mineral synthesis program, aimed at producing actinide-doped REE phosphate EMP dating standards that meet the following criteria: 1) known concentrations of U, Th, and Pb; 2) homogeneous intragrain distribution of all components; 3) of suitable size, either as a single-crystal or polycrystalline sintered ceramic. Single-crystal synthesis of actinide-doped LaPO4 by flux-growth methods results in disproportionation of lanthanide and flux, alkali, and actinide components into phosphate and oxide phases, respectively, and flux- growth methods were abandoned. Actinide-doped La phosphate is successfully prepared by high-T annealing and hydrothermal processing of microcrystalline phosphate; both homogeneity and charge-balance of (Ca, Th, Pb)-bearing LaPO4 increase with increasing solvent acidity during cold-seal hydrothermal synthesis. A combination of pressing and high-T (1400° C) sintering transforms fine-grained (0.1-10 μm) run- products to ceramic pellets with 90-95% theoretical density. Our most recent runs focused on a target composition of La80(CaTh)17(CaU)2(PbTh)1PO4 processed with 6% 2M HCl at 820° C, 0.75 kbar for 1 week. The run products are 0.1-2 μm crystals identified by XRD as La-actinide phosphate solid solution. 2 μm grains (N=16) give a composition (mean±2 sd) of La79.77(1.26)(CaTh)17.87(1.00)(CaU)1.53(0.42)(PbTh)0.82(0.09)PO4. Th (8.07-9.13 wt. %) is homogeneous at the level of analytical precision, and the Pb concentration range (3500-4350 ppm) is restricted relative to untreated precipitate. Uranium concentration values are more variable (6500-10000 ppm). This run yields a fictive age of 702±4 Ma (mean±2 se), compared to the fictive age of 794 Ma for the target composition.

Cementless Hydroxyapatite Coated Hip Prostheses

PubMed Central

Herrera, Antonio; Mateo, Jesús; Gil-Albarova, Jorge; Lobo-Escolar, Antonio; Ibarz, Elena; Gabarre, Sergio; Más, Yolanda

2015-01-01

More than twenty years ago, hydroxyapatite (HA), calcium phosphate ceramics, was introduced as a coating for cementless hip prostheses. The choice of this ceramic is due to its composition being similar to organic apatite bone crystals. This ceramic is biocompatible, bioactive, and osteoconductive. These qualities facilitate the primary stability and osseointegration of implants. Our surgical experience includes the implantation of more than 4,000 cementless hydroxyapatite coated hip prostheses since 1990. The models implanted are coated with HA in the acetabulum and in the metaphyseal area of the stem. The results corresponding to survival and stability of implants were very satisfactory in the long-term. From our experience, HA-coated hip implants are a reliable alternative which can achieve long term survival, provided that certain requirements are met: good design selection, sound choice of bearing surfaces based on patient life expectancy, meticulous surgical technique, and indications based on adequate bone quality. PMID:25802848

Study on ceramic coating on the enamel surface using a carbon dioxide laser.

PubMed

Nihei, Tomotaro; Kurata, Shigeaki; Ohashi, Katsura; Umemoto, Kozo; Teranaka, Toshio

2011-01-01

The aims of this study were to evaluate a new restorative method using a carbon dioxide laser (CO(2)-laser) and to evaluate the acid resistance of teeth. Experimental calcium phosphate glass (CPG) powder and two low melting point ceramics (Finesse and zirconium silicate) were fused to enamel surfaces using a CO(2)-laser at an irradiation intensity of 1.0 watt for 30 seconds with a beam size of 0.49 mm at the focal point. The treated teeth were observed with a scanning electron microscope, and the acid resistance of the treated enamel surfaces was evaluated. The CPG fused successfully to the enamel surface, and the treated enamel surface showed high acid resistance compared with the low melting point ceramics and the non-irradiated surfaces. This system may lead to the development of new restorative methods that do not require the use of bonding agents.

[A study on alpha-tricalcium phosphate bone cement carbon fiber-reinforced].

PubMed

Wu, Wenjin; Yang, Weizhong; Zhou, Dali; Ma, Jiang; Xiao, Bin

2006-06-01

In order to improve the mechanical properties of alpha-tricalcium phosphate (alpha-TCP), we prepared surface-modified carbon fibers (CF) reinforced alpha-TCP composite bone cement. Bone cement was soaked in Ringer's body solution to test its capacity of fast formation of hydroxyapatite crystals and self-solidification. Scan electronic microscope (SEM) observation and compressive strength measurement were taken to analyze the mechanical properties and the micro- morphological structure of CF reinforced alpha-TCP bone cement. The results showed that the bone cement was transferred into hydroxyapatite plates after being soaked in Ringer's simulated body fluid for 5 days. Suitable amount of carbon fibers could well spread in and bond with the matrix of the bone cement. The mechanical properties of the bone cement have been improved by CF reinforcing; the compressive strength reaches 46.7 MPa when the amount of carbon fibers is 0.5% in weight percent, which is 22% higher than that of the non-reinforced alpha-TCP bone cement.

Effect of Luting Cements On the Bond Strength to Turkom-Cera All-Ceramic Material

PubMed Central

Al–Makramani, Bandar M. A.; Razak, Abdul A. A.; Abu–Hassan, Mohamed I.; Al–Sanabani, Fuad A.; Albakri, Fahad M.

2018-01-01

BACKGROUND: The selection of the appropriate luting cement is a key factor for achieving a strong bond between prepared teeth and dental restorations. AIM: To evaluate the shear bond strength of Zinc phosphate cement Elite, glass ionomer cement Fuji I, resin-modified glass ionomer cement Fuji Plus and resin luting cement Panavia-F to Turkom-Cera all-ceramic material. MATERIALS AND METHODS: Turkom-Cera was used to form discs 10mm in diameter and 3 mm in thickness (n = 40). The ceramic discs were wet ground, air - particle abraded with 50 - μm aluminium oxide particles and randomly divided into four groups (n = 10). The luting cement was bonded to Turkom-Cera discs as per manufacturer instructions. The shear bond strengths were determined using the universal testing machine at a crosshead speed of 0.5 mm/min. The data were analysed using the tests One Way ANOVA, the nonparametric Kruskal - Wallis test and Mann - Whitney Post hoc test. RESULTS: The shear bond strength of the Elite, Fuji I, Fuji Plus and Panavia F groups were: 0.92 ± 0.42, 2.04 ± 0.78, 4.37 ± 1.18, and 16.42 ± 3.38 MPa, respectively. There was the statistically significant difference between the four luting cement tested (p < 0.05). CONCLUSION: the phosphate-containing resin cement Panavia-F exhibited shear bond strength value significantly higher than all materials tested. PMID:29610618

Numerical modeling of materials processes with fluid-fluid interfaces

NASA Astrophysics Data System (ADS)

Yanke, Jeffrey Michael

A numerical model has been developed to study material processes that depend on the interaction between fluids with a large discontinuity in thermophysical properties. A base model capable of solving equations of mass, momentum, energy conservation, and solidification has been altered to enable tracking of the interface between two immiscible fluids and correctly predict the interface deformation using a volume of fluid (VOF) method. Two materials processes investigated using this technique are Electroslag Remelting (ESR) and plasma spray deposition. ESR is a secondary melting technique that passes an AC current through an electrically resistive slag to provide the heat necessary to melt the alloy. The simulation tracks the interface between the slag and metal. The model was validated against industrial scale ESR ingots and was able to predict trends in melt rate, sump depth, macrosegregation, and liquid sump depth. In order to better understand the underlying physics of the process, several constant current ESR runs simulated the effects of freezing slag in the model. Including the solidifying slag in the imulations was found to have an effect on the melt rate and sump shape but there is too much uncertainty in ESR slag property data at this time for quantitative predictions. The second process investigated in this work is the deposition of ceramic coatings via plasma spray deposition. In plasma spray deposition, powderized coating material is injected into a plasma that melts and carries the powder towards the substrate were it impacts, flattening out and freezing. The impacting droplets pile up to form a porous coating. The model is used to simulate this rain of liquid ceramic particles impacting the substrate and forming a coating. Trends in local solidification time and porosity are calculated for various particle sizes and velocities. The predictions of decreasing porosity with increasing particle velocity matches previous experimental results. Also, a preliminary study was conducted to investigate the effects of substrate surface defects and droplet impact angle on the propensity to form columnar porosity.

Tailoring the structure of biphasic calcium phosphate via synthesis procedure

NASA Astrophysics Data System (ADS)

Mansour, S. F.; El-dek, S. I.; Ahmed, M. K.

2017-12-01

Nano calcium phosphate ceramics (CaPC) were synthesized using simple co-precipitation method at different preparation conditions. The selected Ca/P ratio with a variation of pH value lead to formation of dicalcium phosphate dihydrate (DCPD) at pH 5 and 6 while, hydroxyapatite (HAP) nano particles were formed at pH 9 and 12 at room temperature. The crystallite size was in the range of 15-55 nm depending on the obtained crystalline phase. The study displayed variation of decomposition depending on the annealing temperature. The significant note is the different transformation trend of each phase depending on the starting pH value. The HRTEM illustrated that the DCPD phase was formed as fibers with diameter around 4-6 nm, while HAP was formed in rod shape. The aspect ratio decreased from 6.6 at pH 9 to 4 at pH 12 which refer to the great influence of pH value on the morphology of calcium phosphates.

Mechanical properties of calcium phosphate scaffolds fabricated by robocasting.

PubMed

Miranda, Pedro; Pajares, Antonia; Saiz, Eduardo; Tomsia, Antoni P; Guiberteau, Fernando

2008-04-01

The mechanical behavior under compressive stresses of beta-tricalcium phosphate (beta-TCP) and hydroxyapatite (HA) scaffolds fabricated by direct-write assembly (robocasting) technique is analyzed. Concentrated colloidal inks prepared from beta-TCP and HA commercial powders were used to fabricate porous structures consisting of a 3-D tetragonal mesh of interpenetrating ceramic rods. The compressive strength and elastic modulus of these model scaffolds were determined by uniaxial testing to compare the relative performance of the selected materials. The effect of a 3-week immersion in simulated body fluid (SBF) on the strength of the scaffolds was also analyzed. The results are compared with those reported in the literature for calcium phosphate scaffolds and human bone. The robocast calcium phosphate scaffolds were found to exhibit excellent mechanical performances in terms of strength, especially the HA structures after SBF immersion, indicating a great potential of this type of scaffolds for use in load-bearing bone tissue engineering applications. Copyright 2007 Wiley Periodicals, Inc.

Studying metal impurities (Mn2+, Cu2+, Fe3+) in calcium phosphates by electron paramagnetic resonance

NASA Astrophysics Data System (ADS)

Iskhakova, K.; Murzakhanov, F.; Mamin, G.; Putlyaev, V.; Klimashina, E.; Fadeeva, I.; Fomin, A.; Barinov, S.; Maltsev, A.; Bakhteev, S.; Yusupov, R.; Gafurov, M.; Orlinskii, S.

2018-05-01

Calcium phosphates (CaP) are exploited in many fields of science, including geology, chemistry, biology and medicine due to their abundance in the nature and presence in the living organism. Various analytical and biochemical methods are used for controlling their chemical content, structure, morphology, etc. Unfortunately, magnetic resonance techniques are usually not even considered as necessary tools for CaP inspection. Some aspects of application of the commercially realized electron paramagnetic resonance (EPR) approaches for characterization of CaP powders and ceramics (including the nanosized materails) such as hydroxyapatite and tricalcium phosphates of biogenic and synthetic origins containing intrinsic impurities or intentional dopants are demonstrated. The key features and advantages of the EPR techniques for CaP based materials characterization that could compliment the data obtained with the recognized analytical methods are pointed out.

Bond strength of selected composite resin-cements to zirconium-oxide ceramic

PubMed Central

Fons-Font, Antonio; Amigó-Borrás, Vicente; Granell-Ruiz, María; Busquets-Mataix, David; Panadero, Rubén A.; Solá-Ruiz, Maria F.

2013-01-01

Objectives: The aim of this study was to evaluate bond strengths of zirconium-oxide (zirconia) ceramic and a selection of different composite resin cements. Study Design: 130 Lava TM cylinders were fabricated. The cylinders were sandblasted with 80 µm aluminium oxide or silica coated with CoJet Sand. Silane, and bonding agent and/or Clearfil Ceramic Primer were applied. One hundred thirty composite cement cylinders, comprising two dual-polymerizing (Variolink II and Panavia F) and two autopolymerizing (Rely X and Multilink) resins were bonded to the ceramic samples. A shear test was conducted, followed by an optical microscopy study to identify the location and type of failure, an electron microscopy study (SEM and TEM) and statistical analysis using the Kruskal-Wallis test for more than two independent samples and Mann-Whitney for two independent samples. Given the large number of combinations, Bonferroni correction was applied (α=0.001). Results: Dual-polymerizing cements provided better adhesion values (11.7 MPa) than the autopolymerizing (7.47 MPa) (p-value M-W<0.001). The worst techniques were Lava TM + sandblasting + Silane + Rely X; Lava TM + sandblasting + Silane + Multilink and Lava TM + CoJet + silane + Multilink. Adhesive failure (separation of cement and ceramic) was produced at a lesser force than cohesive failure (fracture of cement) (p-value M-W<0.001). Electron microscopy confirmed that the surface treatments modified the zirconium-oxide ceramic, creating a more rough and retentive surface, thus providing an improved micromechanical interlocking between the cement and the ceramic. Key words:Shear bond strength, silica coating, surface treatment, zirconia ceramics, phosphate monomer. PMID:22926485

Development of an external ceramic insulation for the space shuttle orbiter. Part 3: Development of stabilized aluminum phosphate fibers

NASA Technical Reports Server (NTRS)

Ormiston, T.; Tanzilli, R. A.

1973-01-01

The development of reusable surface insulation materials that are thermal shock resistant and highly refractory is discussed. A stabilized, high-cristobalite, aluminum orthophosphate fiber was developed and found to possess the desired qualities. The application of such a material to heat shielding for space shuttles is examined.

Vertical marginal discrepancy of ceramic copings with different ceramic materials, finish lines, and luting agents: an in vitro evaluation.

PubMed

Quintas, Adriana Ferreira; Oliveira, Fabiano; Bottino, Marco Antonio

2004-09-01

Prosthetic restorations that fit poorly may affect periodontal health and occlusion. Studies that have evaluated the accuracy of fit of ceramic restorations before and after cementation assessed primarily intracoronal restorations. This in vitro study evaluated the effect of different finish lines, ceramic manufacturing techniques, and luting agents on the vertical discrepancy of ceramic copings. Two stainless steel molars were prepared for complete crowns with 2 different finish lines (heavy chamfer and rounded shoulder); each molar was duplicated to fabricate 90 copings. A total of 180 copings generated 18 groups (n=10 for each finish line-coping material-luting agent combination). Luting agents tested included zinc phosphate, resin-modified glass ionomer (Fuji Plus), and resin composite cements (Panavia F). A metal frame was developed on which to screw the stainless steel model and a ceramic coping; the distance (microm) between 2 predetermined points was measured before and after cementation by a profile projector under a torquing force. A 4-way ANOVA with repeated measurements was performed to assess the influence of each factor in the vertical marginal discrepancy: 3 between-coping factors (finish line-coping material-luting agent) and 1 within-coping factor (before and after cementation) (alpha=.05). Procera copings presented the lowest mean values ( P <.05) of vertical marginal discrepancy before and after cementation (25/44 microm) when compared to Empress 2 (68/110 microm) and InCeram Alumina copings (57/117 microm), regardless of any combinations among all finish lines and luting agents tested. Considering each factor separately, the ceramic manufacturing technique appeared to be the most important factor tested for the definitive vertical discrepancy of all-ceramic copings, with lower mean values for Procera copings.

In vitro and in vivo study of microporous ceramics using MC3T3 cells, CAM assay and a pig animal model.

PubMed

Tomco, Marek; Petrovova, Eva; Giretova, Maria; Almasiova, Viera; Holovska, Katarina; Cigankova, Viera; Jenca, Andrej; Jencova, Janka; Jenca, Andrej; Boldizar, Martin; Balazs, Kosa; Medvecky, Lubomir

2017-09-01

Bone tissue engineering combines biomaterials with biologically active factors and cells to hold promise for reconstructing craniofacial defects. In this study the biological activity of biphasic hydroxyapatite ceramics (HA; a bone substitute that is a mixture of hydroxyapatite and β-tricalcium phosphate in fixed ratios) was characterized (1) in vitro by assessing the growth of MC3T3 mouse osteoblast lineage cells, (2) in ovo by using the chick chorioallantoic membrane (CAM) assay and (3) in an in vivo pig animal model. Biocompatibility, bioactivity, bone formation and biomaterial degradation were detected microscopically and by radiology and histology. HA ceramics alone demonstrated great biocompatibility on the CAM as well as bioactivity by increased proliferation and alkaline phosphatase secretion of mouse osteoblasts. The in vivo implantation of HA ceramics with bone marrow mesenchymal stem cells (MMSCs) showed de novo intramembranous bone healing of critical-size bone defects in the right lateral side of pig mandibular bodies after 3 and 9 weeks post-implantation. Compared with the HA ceramics without MMSCs, the progress of bone formation was slower with less-developed features. This article highlights the clinical use of microporous biphasic HA ceramics despite the unusually shaped elongated micropores with a high length/width aspect ratio (up to 20) and absence of preferable macropores (>100 µm) in bone regenerative medicine.

Design and Characterization of Calcium Phosphate Ceramic Scaffolds for Bone Tissue Engineering

PubMed Central

Kuhn, Liisa T.

2015-01-01

Objectives Our goal is to review design strategies for the fabrication of calcium phosphate ceramic scaffolds (CPS), in light of their transient role in bone tissue engineering and associated requirements for effective bone regeneration. Methods We examine the various design options available to meet mechanical and biological requirements of CPS and later focus on the importance of proper characterization of CPS in terms of architecture, mechanical properties and time-sensitive properties such as biodegradability. Finally, relationships between in vitro vs. in vivo testing are addressed, with an attempt to highlight reliable performance predictors. Results A combinatory design strategy should be used with CPS taking into consideration 3D architecture, adequate surface chemistry and topography, all of which are needed to promote bone formation. CPS represent the media of choice for delivery of osteogenic factors and anti-infectives. Non-osteoblast mediated mineral deposition can confound in vitro osteogenesis testing of CPS and therefore the expression of a variety of proteins or genes including collagen type I, bone sialoprotein and osteocalcin should be confirmed in addition to increased mineral content. Conclusions CPS are a superior scaffold material for bone regeneration because they actively promote osteogenesis. Biodegradability of CPS via calcium and phosphate release represents a unique asset. Structural control of CPS at the macro, micro and nanoscale and their combination with cells and polymeric materials is likely to lead to significant developments in bone tissue engineering. PMID:26423007

Design and characterization of calcium phosphate ceramic scaffolds for bone tissue engineering.

PubMed

Denry, Isabelle; Kuhn, Liisa T

2016-01-01

Our goal is to review design strategies for the fabrication of calcium phosphate ceramic scaffolds (CPS), in light of their transient role in bone tissue engineering and associated requirements for effective bone regeneration. We examine the various design options available to meet mechanical and biological requirements of CPS and later focus on the importance of proper characterization of CPS in terms of architecture, mechanical properties and time-sensitive properties such as biodegradability. Finally, relationships between in vitro versus in vivo testing are addressed, with an attempt to highlight reliable performance predictors. A combinatory design strategy should be used with CPS, taking into consideration 3D architecture, adequate surface chemistry and topography, all of which are needed to promote bone formation. CPS represent the media of choice for delivery of osteogenic factors and anti-infectives. Non-osteoblast mediated mineral deposition can confound in vitro osteogenesis testing of CPS and therefore the expression of a variety of proteins or genes including collagen type I, bone sialoprotein and osteocalcin should be confirmed in addition to increased mineral content. CPS are a superior scaffold material for bone regeneration because they actively promote osteogenesis. Biodegradability of CPS via calcium and phosphate release represents a unique asset. Structural control of CPS at the macro, micro and nanoscale and their combination with cells and polymeric materials is likely to lead to significant developments in bone tissue engineering. Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Osteoconduction of impacted porous titanium particles with a calcium-phosphate coating is comparable to osteoconduction of impacted allograft bone particles: in vivo study in a nonloaded goat model.

PubMed

Walschot, Lucas H B; Aquarius, René; Schreurs, Barend W; Verdonschot, Nico; Buma, Pieter

2012-08-01

Impaction grafting restores bone defects in hip arthroplasty. Defects are reconstructed with bone particles (BoP) as substitute materials with adequate mechanical and biological properties are not yet available. Ceramic particles (CeP) have mechanical drawbacks as opposed to porous titanium particles (TiP). In this in vivo study, bone ingrowth and bone volume in coated and noncoated TiP were compared to porous biphasic calcium-phospate CeP and allograft BoP. Coatings consisted of silicated calcium-phosphate and carbonated apatite. Materials were implanted in goats and impacted in cylindrical defects (diameter 8 mm) in the cancellous bone of the femur. On the basis of fluorochrome labeling and histology, bone ingrowth distance was measured at 4, 8, and 12 weeks. Cross-sectional bone area was measured at 12 weeks. TiP created a coherent matrix of entangled particles. CeP pulverized and were noncoherent. Bone ingrowth in TiP improved significantly by the coatings to levels comparable to BoP and CeP. Cross-sectional bone area was smaller in CeP and TiP compared to BoP. The osteoconductive properties of impacted TiP with a calcium-phosphate coating are comparable to impacted allograft bone and impacted biphasic ceramics. A more realistic loaded in vivo study should prove that coated TiP is an attractive alternative to allograft bone. Copyright © 2012 Wiley Periodicals, Inc.

The effect of rotating magnetic field on the microstructure of in situ TiB2/Cu composites

NASA Astrophysics Data System (ADS)

Zou, C.; Kang, H.; Li, R.; Li, M.; Wang, W.; Chen, Z.; Wang, T.

2016-03-01

Nano ceramic particulate reinforced metal matrix composites are confronted with the problem of particle aggregation emerging in the process of solidification. It sharply deteriorates the mechanical properties of the composites. In order to improve the microstructure and particle distribution, in situ TiB2/Cu composites were prepared using Ti and Cu-B master alloys in a vacuum medium frequency induction furnace equipped with a rotating magnetic field (RMF). The effect of RMF magnetic field intensity employed on the microstructure and particles distribution of the TiB2/Cu composites were investigated. The results show that with the applied RMF, TiB2 particles are homogeneously distributed in the copper matrix, which significantly improves the mechanical properties of TiB2/Cu composites. The mechanism of RMF may be ascribed to the following two aspects. On the one hand, the electromagnetic body force generated by appropriate RMF drives forced convection in the equatorial plane of composite melt during solidification. On the other hand, a secondary flow in the meridional plane is engendered by a radial pressure gradient, thus making a strong agitation in the melt. These two effects result in a homogenous dispersion of TiB2 particles in the copper matrix, and hence excellent properties of TiB2/Cu composites were obtained.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ivanov, Yuri, E-mail: yufi55@mail.ru; National Research Tomsk State University, 36 Lenina Str., Tomsk, 634050; National Research Tomsk Polytechnic University, 30 Lenina Str., Tomsk, 634050

The present work is devoted to numerical simulation of temperature fields and the analysis of structural and strength properties of the samples surface layer of boron carbide ceramics treated by the high-current pulsed electron-beam of the submillisecond duration. The samples made of sintered boron carbide ceramics are used in these investigations. The problem of calculating the temperature field is reduced to solving the thermal conductivity equation. The electron beam density ranges between 8…30 J/cm{sup 2}, while the pulse durations are 100…200 μs in numerical modelling. The results of modelling the temperature field allowed ascertaining the threshold parameters of the electronmore » beam, such as energy density and pulse duration. The electron beam irradiation is accompanied by the structural modification of the surface layer of boron carbide ceramics either in the single-phase (liquid or solid) or two-phase (solid-liquid) states. The sample surface of boron carbide ceramics is treated under the two-phase state (solid-liquid) conditions of the structural modification. The surface layer is modified by the high-current pulsed electron-beam produced by SOLO installation at the Institute of High Current Electronics of the Siberian Branch of the Russian Academy of Sciences, Tomsk, Russia. The elemental composition and the defect structure of the modified surface layer are analyzed by the optical instrument, scanning electron and transmission electron microscopes. Mechanical properties of the modified layer are determined measuring its hardness and crack resistance. Research results show that the melting and subsequent rapid solidification of the surface layer lead to such phenomena as fragmentation due to a crack network, grain size reduction, formation of the sub-grained structure due to mechanical twinning, and increase of hardness and crack resistance.« less

Heat treatment of pre-hydrolyzed silane increases adhesion of phosphate monomer-based resin cement to glass ceramic.

PubMed

de Carvalho, Rodrigo Furtado; Cotes, Caroline; Kimpara, Estevão Tomomitsu; Leite, Fabíola Pessoa Pereira; Özcan, Mutlu

2015-01-01

This study evaluated the influence of different forms of heat treatment on a pre-hydrolyzed silane to improve the adhesion of phosphate monomer-based (MDP) resin cement to glass ceramic. Resin and feldspathic ceramic blocks (n=48, n=6 for bond test, n=2 for microscopy) were randomly divided into 6 groups and subject to surface treatments: G1: Hydrofluoric acid (HF) 9.6% for 20 s + Silane + MDP resin cement (Panavia F); G2: HF 9.6% for 20 s + Silane + Heat Treatment (oven) + Panavia F; G3: Silane + Heat Treatment (oven) + Panavia F; G4: HF 9.6% for 20 s + Silane + Heat Treatment (hot air) + Panavia F; G5: Silane + Heat Treatment (hot air) + Panavia F; G6: Silane + Panavia F. Microtensile bond strength (MTBS) test was performed using a universal testing machine (1 mm/min). After debonding, the substrate and adherent surfaces were analyzed using stereomicroscope and scanning electron microscope (SEM) to categorize the failure types. Data were analyzed statistically using two-way test ANOVA and Tukey's test (=0.05). Heat treatment of the silane containing MDP, with prior etching with HF (G2: 13.15 ± 0.89a; G4: 12.58 ± 1.03a) presented significantly higher bond strength values than the control group (G1: 9.16 ± 0.64b). The groups without prior etching (G3: 10.47 ± 0.70b; G5: 9.47 ± 0.32b) showed statistically similar bond strength values between them and the control group (G1). The silane application without prior etching and heat treatment resulted in the lowest mean bond strength (G6: 8.05 ± 0.37c). SEM analysis showed predominantly adhesive failures and EDS analysis showed common elements of spectra (Si, Na, Al, K, O, C) characterizing the microstructure of the glass-ceramic studied. Heat treatment of the pre-hydrolyzed silane containing MDP in an oven at 100 °C for 2 min or with hot air application at 50 ± 5 ºC for 1 min, was effective in increasing the bond strength values between the ceramic and resin cement containing MDP.

Effect of nano-hydroxyapatite coating on the osteoinductivity of porous biphasic calcium phosphate ceramics.

PubMed

Hu, Jianzhong; Zhou, Yongchun; Huang, Lihua; Liu, Jun; Lu, Hongbin

2014-04-01

Porous biphasic calcium phosphate (BCP) ceramics exhibit good biocompatibility and bone conduction but are not inherently osteoinductive. To overcome this disadvantage, we coated conventional porous BCP ceramics with nano-hydroxyapatite (nHA). nHA was chosen as a coating material due to its high osteoinductive potential. We used a hydrothermal deposition method to coat conventional porous BCP ceramics with nHA and assessed the effects of the coating on the physical and mechanical properties of the underlying BCP. Next, its effects on mesenchymal stem cell (MSC) attachment, proliferation, viability, and osteogenic differentiation were investigated. nHA formed a deposited layer on the BCP surface, and synthesized nHA had a rod-like shape with lengths ranging from ~50-200 nm and diameters from ~15-30 mm. The nHA coating did not significantly affect the density, porosity, flexural strength, or compressive strength of the underlying BCP (P > 0.1). Scanning electron microscopy showed MSC attachment to the scaffolds, with a healthy morphology and anchorage to nHA crystals via cytoplasmic processes. The densities of MSCs attached on BCP and nHA-coated BCP scaffolds were 62 ± 26 cells/mm2 and 63 ± 27 cells/mm2 (P > 0.1), respectively, after 1 day and 415 ± 62 cells/mm2 and 541 ± 35 cells/mm2 (P < 0.05) respectively, after 14 days. According to an MTT assay, MSC viability was higher on nHA-coated BCP scaffolds than on BCP scaffolds (P < 0.05). In addition, MSCs on nHA-coated BCP scaffolds produced more alkaline phosphatase, collagen type I, and osteocalcin than MSCs on BCP scaffolds (P < 0.05). Our results demonstrate that BCP scaffolds coated with nHA were more conducive for MSC adhesion, proliferation, and osteogenic differentiation than conventional, uncoated BCP scaffolds, indicating that nHA coating can enhance the osteoinductive potential of BCP ceramics, making this material more suitable for applications in bone tissue engineering.

Effect of nano-hydroxyapatite coating on the osteoinductivity of porous biphasic calcium phosphate ceramics

PubMed Central

2014-01-01

Background Porous biphasic calcium phosphate (BCP) ceramics exhibit good biocompatibility and bone conduction but are not inherently osteoinductive. To overcome this disadvantage, we coated conventional porous BCP ceramics with nano-hydroxyapatite (nHA). nHA was chosen as a coating material due to its high osteoinductive potential. Methods We used a hydrothermal deposition method to coat conventional porous BCP ceramics with nHA and assessed the effects of the coating on the physical and mechanical properties of the underlying BCP. Next, its effects on mesenchymal stem cell (MSC) attachment, proliferation, viability, and osteogenic differentiation were investigated. Results nHA formed a deposited layer on the BCP surface, and synthesized nHA had a rod-like shape with lengths ranging from ~50–200 nm and diameters from ~15–30 mm. The nHA coating did not significantly affect the density, porosity, flexural strength, or compressive strength of the underlying BCP (P > 0.1). Scanning electron microscopy showed MSC attachment to the scaffolds, with a healthy morphology and anchorage to nHA crystals via cytoplasmic processes. The densities of MSCs attached on BCP and nHA-coated BCP scaffolds were 62 ± 26 cells/mm2 and 63 ± 27 cells/mm2 (P > 0.1), respectively, after 1 day and 415 ± 62 cells/mm2 and 541 ± 35 cells/mm2 (P < 0.05) respectively, after 14 days. According to an MTT assay, MSC viability was higher on nHA-coated BCP scaffolds than on BCP scaffolds (P < 0.05). In addition, MSCs on nHA-coated BCP scaffolds produced more alkaline phosphatase, collagen type I, and osteocalcin than MSCs on BCP scaffolds (P < 0.05). Conclusions Our results demonstrate that BCP scaffolds coated with nHA were more conducive for MSC adhesion, proliferation, and osteogenic differentiation than conventional, uncoated BCP scaffolds, indicating that nHA coating can enhance the osteoinductive potential of BCP ceramics, making this material more suitable for applications in bone tissue engineering. PMID:24690170

Survey Analysis of Materials Processing Experiments Aboard STS-47: Spacelab J

NASA Technical Reports Server (NTRS)

Sharpe, R. J.; Wright, M. D.

2009-01-01

This Technical Memorandum (TM) is a survey outline of materials processing experiments aboard Space Shuttle Mission STS-47: Spacelab J, a joint venture between NASA and the National Space Development Agency of Japan. The mission explored materials processing experiments including electronics and crystal growth materials, metals and alloys, glasses and ceramics, and fluids. Experiments covered include Growth of Silicone Spherical Crystals and Surface Oxidation, Growth Experiment of Narrow Band-Gap Semiconductor Lead-Tin-Tellurium Crystals in Space, Study on Solidification of Immiscible Alloys, Fabrication of Very-Low-Density, High-Stiffness Carbon Fiber/Aluminum Hybridized Composites, High Temperature Behavior of Glass, and Study of Bubble Behavior. The TM underscores the historical significance of these experiments in the context of materials processing in space.

Microgravity science and applications program tasks, 1991 revision

NASA Technical Reports Server (NTRS)

1992-01-01

Presented here is a compilation of the active research tasks for FY 1991 sponsored by the Microgravity Science and Applications Division of the NASA Office of Space Science and Applications. The purpose is to provide an overview of the program scope for managers and scientists in industry, university, and government communities. Included is an introductory description of the program, the strategy and overall goal, identification of the organizational structures and the people involved, and a description of each. The tasks are grouped into several categories: electronic materials; solidification of metals, alloys, and composites; fluids, interfaces, and transport; biotechnology; combustion science; glasses and ceramics; experimental technology, instrumentation, and facilities; and Physical and Chemistry Experiments (PACE). The tasks cover both the ground based and flight programs.

A Process for Manufacturing Metal-Ceramic Cellular Materials with Designed Mesostructure

NASA Astrophysics Data System (ADS)

Snelling, Dean Andrew, Jr.

The goal of this work is to develop and characterize a manufacturing process that is able to create metal matrix composites with complex cellular geometries. The novel manufacturing method uses two distinct additive manufacturing processes: i) fabrication of patternless molds for cellular metal castings and ii) printing an advanced cellular ceramic for embedding in a metal matrix. However, while the use of AM greatly improves the freedom in the design of MMCs, it is important to identify the constraints imposed by the process and its process relationships. First, the author investigates potential differences in material properties (microstructure, porosity, mechanical strength) of A356 - T6 castings resulting from two different commercially available Binder Jetting media and traditional "no-bake" silica sand. It was determined that they yielded statistically equivalent results in four of the seven tests performed: dendrite arm spacing, porosity, surface roughness, and tensile strength. They differed in sand tensile strength, hardness, and density. Additionally, two critical sources of process constraints on part geometry are examined: (i) depowdering unbound material from intricate casting channels and (ii) metal flow and solidification distances through complex mold geometries. A Taguchi Design of Experiments is used to determine the relationships of important independent variables of each constraint. For depowdering, a minimum cleaning diameter of 3 mm was determined along with an equation relating cleaning distance as a function of channel diameter. Furthermore, for metal flow, choke diameter was found to be significantly significant variable. Finally, the author presents methods to process complex ceramic structure from precursor powders via Binder Jetting AM technology to incorporate into a bonded sand mold and the subsequently casted metal matrix. Through sintering experiments, a sintering temperature of 1375°C was established for the ceramic insert (78% cordierite). Upon printing and sintering the iii ceramic, three point bend tests showed the MMCs had less strength than the matrix material likely due to the relatively high porosity developed in the body. Additionally, it was found that the ceramic metal interface had minimal mechanical interlocking and chemical bonding limiting the strength of the final MMCs.

Proliferation and osteoblastic differentiation of human bone marrow-derived stromal cells on akermanite-bioactive ceramics.

PubMed

Sun, Hongli; Wu, Chengtie; Dai, Kerong; Chang, Jiang; Tang, Tingting

2006-11-01

In the present study, the effects of a calcium magnesium silicate bioactive ceramic (akermanite) on proliferation and osteoblastic differentiation of human bone marrow stromal cells (hBMSC) have been investigated and compared with the classical ceramic (beta-tricalcium phosphate, beta-TCP). Akermanite and beta-TCP disks were seeded with hBMSC and kept in growth medium or osteogenic medium for 10 days. Proliferation and osteoblastic differentiation were evaluated on day 1, 4, 7 and 10. The data from the Alamar Blue assay and lactic acid production assay showed that hBMSC proliferated more significantly on akermanite than on beta-TCP. The analysis of osteoblast-related genes, including alkaline phosphatase (ALP), osteopontin (OPN), bone sialoprotein (BSP) and osteocalcin (OC), indicated that akermanite ceramics enhanced the expression of osteoblast-related genes, but type I collagen (COL I) showed no noticeable difference among akermanite and beta-TCP ceramics. Furthermore, this stimulatory effect was observed not only in osteogenic medium, but also in normal growth medium without osteogenic reagents such as l-ascorbic acid, glycerophosphate and dexamethasone. This result suggests that akermanite can promote osteoblastic differentiation of hBMSC in vitro even without osteogenic reagents, and may be used as a bioactive material for bone regeneration and tissue engineering applications.

Poly(trimethylene carbonate)-based composite materials for reconstruction of critical-sized cranial bone defects in sheep.

PubMed

Zeng, Ni; van Leeuwen, Anne C; Grijpma, Dirk W; Bos, Ruud R M; Kuijer, Roel

2017-02-01

The use of ceramic materials in repair of bone defects is limited to non-load-bearing sites. We tested poly(trimethylene carbonate) (PTMC) combined with β-tricalcium phosphate or biphasic calcium phosphate particles for reconstruction of cranial defects. PTMC-calcium phosphate composite matrices were implanted in cranial defects in sheep for 3 and 9 months. Micro-computed tomography quantification and histological observation were performed for analysis. No differences were found in new bone formation among the defects left unfilled, filled with PTMC scaffolds, or filled with either kind of PTMC-calcium phosphate composite scaffolds. Porous β-TCP scaffolds as control led to a larger amount of newly formed bone in the defects than all other materials. Histology revealed abundant new bone formation in the defects filled with porous β-TCP scaffolds. New bone formation was limited in defects filled with PTMC scaffolds or different PTMC-calcium phosphate matrices. PTMC matrices were degraded uneventfully. New bone formation within the defects followed an orderly pattern. PTMC did not interfere with bone regeneration in sheep cranial defects and is suitable as a polymer matrix for incorporating calcium phosphate particles. Increasing the content of calcium phosphate particles in the composite matrices may enhance the beneficial effects of the particles on new bone formation. Copyright © 2016 European Association for Cranio-Maxillo-Facial Surgery. Published by Elsevier Ltd. All rights reserved.

3D Printing of Calcium Phosphate Ceramics for Bone Tissue Engineering and Drug Delivery

PubMed Central

Trombetta, Ryan; Inzana, Jason A.; Schwarz, Edward M.; Kates, Stephen L.; Awad, Hani A.

2016-01-01

Additive manufacturing, also known as 3D printing, has emerged over the past 3 decades as a disruptive technology for rapid prototyping and manufacturing. Vat polymerization, powder bed fusion, material extrusion, and binder jetting are distinct technologies of additive manufacturing, which have been used in a wide variety of fields, including biomedical research and tissue engineering. The ability to print biocompatible, patient-specific geometries with controlled macro- and micropores, and to incorporate cells, drugs and proteins has made 3D-printing ideal for orthopaedic applications, such as bone grafting. Herein, we performed a systematic review examining the fabrication of calcium phosphate (CaP) ceramics by 3D printing, their biocompatibility in vitro, and their bone regenerative potential in vivo, as well as their use in localized delivery of bioactive molecules or cells. Understanding the advantages and limitations of the different 3D printing approaches, CaP materials, and bioactive additives through critical evaluation of in vitro and in vivo evidence of efficacy is essential for developing new classes of bone graft substitutes that can perform as well as autografts and allografts or even surpass the performance of these clinical standards. PMID:27324800

Mercury stabilization in chemically bonded phosphate ceramics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wagh, Arun S.; Jeong, Seung-Young; Singh, Dileep

1997-07-01

We have investigated mercury stabilization in chemically bonded phosphate ceramic (CBPC) using four surrogate waste streams that represent U.S. Department of Energy (DOE) ash, soil, and two secondary waste streams resulting from the destruction of DOE`s high-organic wastes by the DETOX{sup SM} Wet Oxidation Process. Hg content in the waste streams was 0.1 to 0.5 wt.% (added as soluble salts). Sulfidation of Hg and its concurrent stabilization in the CBPC matrix yielded highly nonleachable waste forms. The Toxicity Characteristic Leaching Procedure showed that leaching levels were well below the U.S. Environmental Protection Agency`s regulatory limits. The American Nuclear Society`s ANSmore » 16.1 immersion test also gave very high leaching indices, indicating excellent retention of the contaminants. In particular, leaching levels of Hg in the ash waste form were below the measurement detection limit in neutral and alkaline water, negligibly low but measureable in the first 72 h of leaching in acid water, and below the detection limit after that. These studies indicate that the waste forms are stable in a wide range of chemical environments during storage. 9 refs., 5 tabs.« less

3D Printing of Calcium Phosphate Ceramics for Bone Tissue Engineering and Drug Delivery.

PubMed

Trombetta, Ryan; Inzana, Jason A; Schwarz, Edward M; Kates, Stephen L; Awad, Hani A

2017-01-01

Additive manufacturing, also known as 3D printing, has emerged over the past 3 decades as a disruptive technology for rapid prototyping and manufacturing. Vat polymerization, powder bed fusion, material extrusion, and binder jetting are distinct technologies of additive manufacturing, which have been used in a wide variety of fields, including biomedical research and tissue engineering. The ability to print biocompatible, patient-specific geometries with controlled macro- and micro-pores, and to incorporate cells, drugs and proteins has made 3D-printing ideal for orthopaedic applications, such as bone grafting. Herein, we performed a systematic review examining the fabrication of calcium phosphate (CaP) ceramics by 3D printing, their biocompatibility in vitro, and their bone regenerative potential in vivo, as well as their use in localized delivery of bioactive molecules or cells. Understanding the advantages and limitations of the different 3D printing approaches, CaP materials, and bioactive additives through critical evaluation of in vitro and in vivo evidence of efficacy is essential for developing new classes of bone graft substitutes that can perform as well as autografts and allografts or even surpass the performance of these clinical standards.

Biomimetic fabrication of a three-level hierarchical calcium phosphate/collagen/hydroxyapatite scaffold for bone tissue engineering.

PubMed

Zhou, Changchun; Ye, Xingjiang; Fan, Yujiang; Ma, Liang; Tan, Yanfei; Qing, Fangzu; Zhang, Xingdong

2014-09-01

A three-level hierarchical calcium phosphate/collagen/hydroxyapatite (CaP/Col/HAp) scaffold for bone tissue engineering was developed using biomimetic synthesis. Porous CaP ceramics were first prepared as substrate materials to mimic the porous bone structure. A second-level Col network was then composited into porous CaP ceramics by vacuum infusion. Finally, a third-level HAp layer was achieved by biomimetic mineralization. The three-level hierarchical biomimetic scaffold was characterized using scanning electron microscopy, energy-dispersive x-ray spectra, x-ray diffraction and Fourier transform infrared spectroscopy, and the mechanical properties of the scaffold were evaluated using dynamic mechanical analysis. The results show that this scaffold exhibits a similar structure and composition to natural bone tissues. Furthermore, this three-level hierarchical biomimetic scaffold showed enhanced mechanical strength compared with pure porous CaP scaffolds. The biocompatibility and osteoinductivity of the biomimetic scaffolds were evaluated using in vitro and in vivo tests. Cell culture results indicated the good biocompatibility of this biomimetic scaffold. Faster and increased bone formation was observed in these scaffolds following a six-month implantation in the dorsal muscles of rabbits, indicating that this biomimetic scaffold exhibits better osteoinductivity than common CaP scaffolds.

Treatment of phosphate-containing oily wastewater by coagulation and microfiltration.

PubMed

Zhang, Jin; Sun, Yu-xin; Huang, Zhi-feng; Liu, Xing-qin; Meng, Guang-yao

2006-01-01

The oily wastewater generated from pretreatment unit of electrocoating industry contains oils, phosphate, organic solvents, and surfactants. In order to improve the removal efficiencies of phosphate and oils, to mitigate the membrane fouling, coagulation for ceramic membrane microfiltration of oily wastewater was performed. The results of filtration tests show that the membrane fouling decreased and the permeate flux and quality increased with coagulation as pretreatment. At the coagulant Ca (OH)2 dosage of 900 mg/L, the removal efficiency of phosphate was increased from 46.4% without coagulation to 99.6%; the removal of COD and oils were 97.0% and 99.8%, respectively. And the permeate flux was about 70% greater than that when Ca(OH)2 was not used. The permeate obtained from coagulation and microfiltration can be reused as make-up water, and the recommended operation conditions for pilot and industrial application are transmembrane pressure of 0.10 MPa and cross-flow velocity of 5 m/s. The comparison results show that 0.2 microm ZrO2 microfilter with coagulation could be used to perform the filtration rather than conventional ultrafilter, with very substantial gain in flux and removal efficiency of phosphate.

Ceramic Biocomposites as Biodegradable Antibiotic Carriers in the Treatment of Bone Infections

PubMed Central

Ferguson, Jamie; Diefenbeck, Michael; McNally, Martin

2017-01-01

Local release of antibiotic has advantages in the treatment of chronic osteomyelitis and infected fractures. The adequacy of surgical debridement is still key to successful clearance of infection but local antibiotic carriers seem to afford greater success rates by targeting the residual organisms present after debridement and delivering much higher local antibiotic concentrations compared with systemic antibiotics alone. Biodegradable ceramic carriers can be used to fill osseous defects, which reduces the dead space and provides the potential for subsequent repair of the osseous defect as they dissolve away. A dissolving ceramic antibiotic carrier also raises the possibility of single stage surgery with definitive closure and avoids the need for subsequent surgery for spacer removal. In this article we provide an overview of the properties of various biodegradable ceramics, including calcium sulphate, the calcium orthophosphate ceramics, calcium phosphate cement and polyphasic carriers. We summarise the antibiotic elution properties as investigated in previous animal studies as well as the clinical outcomes from clinical research investigating their use in the surgical management of chronic osteomyelitis. Calcium sulphate pellets have been shown to be effective in treating local infection, although newer polyphasic carriers may support greater osseous repair and reduce the risk of further fracture or the need for secondary reconstructive surgery. The use of ceramic biocomposites to deliver antibiotics together with BMPs, bisphosphonates, growth factors or living cells is under investigation and merits further study. We propose a treatment protocol, based on the Cierny-Mader classification, to help guide the appropriate selection of a suitable ceramic antibiotic carrier in the surgical treatment of chronic osteomyelitis. PMID:28529863

Ex vivo and in vitro synchrotron-based micro-imaging of biocompatible materials applied in dental surgery

NASA Astrophysics Data System (ADS)

Rack, A.; Stiller, M.; Nelson, K.; Knabe, C.; Rack, T.; Zabler, S.; Dalügge, O.; Riesemeier, H.; Cecilia, A.; Goebbels, J.

2010-09-01

Biocompatible materials such as porous bioactive calcium phosphate ceramics or titanium are regularly applied in dental surgery: ceramics are used to support the local bone regeneration in a given defect, afterwards titanium implants replace lost teeth. The current gold standard for bone reconstruction in implant dentistry is the use of autogenous bone grafts. But the concept of guided bone regeneration (GBR) has become a predictable and well documented surgical approach using biomaterials (bioactive calcium phosphate ceramics) which qualify as bone substitutes for this kind of application as well. We applied high resolution synchrotron microtomography and subsequent 3d image analysis in order to investigate bone formation and degradation of the bone substitute material in a three-dimensional manner, extending the knowledge beyond the limits of classical histology. Following the bone regeneration, titanium-based implants to replace lost teeth call for high mechanical precision, especially when two-piece concepts are used in order to guaranty leak tightness. Here, synchrotron-based radiography in comparison with classical laboratory radiography yields high spatial resolution in combination with high contrast even when exploiting micro-sized features in these kind of highly attenuating objects. Therefore, we could study micro-gap formation at interfaces in two-piece dental implants with the specimen under different mechanical load. We could prove the existence of micro-gaps for implants with conical connections as well as to study the micromechanical behavior of the mating zone of conical implants during loading. The micro-gap is a potential issue of failure, i. e. bacterial leakage which can induce an inflammatory process.

Coextrusion-Based 3D Plotting of Ceramic Pastes for Porous Calcium Phosphate Scaffolds Comprised of Hollow Filaments.

PubMed

Jo, In-Hwan; Koh, Young-Hag; Kim, Hyoun-Ee

2018-05-29

This paper demonstrates the utility of coextrusion-based 3D plotting of ceramic pastes (CoEx-3DP) as a new type of additive manufacturing (AM) technique, which can produce porous calcium phosphate (CaP) ceramic scaffolds comprised of hollow CaP filaments. In this technique, green filaments with a controlled core/shell structure can be produced by coextruding an initial feedrod, comprised of the carbon black (CB) core and CaP shell, through a fine nozzle in an acetone bath and then deposited in a controlled manner according to predetermined paths. In addition, channels in CaP filaments can be created through the removal of the CB cores during heat-treatment. Produced CaP scaffolds had two different types of pores with well-defined geometries: three-dimensionally interconnected pores (~360 × 230 μm² in sizes) and channels (>100 μm in diameter) in hollow CaP filaments. The porous scaffolds showed high compressive strengths of ~12.3 ± 2.2 MPa at a high porosity of ~73 vol % when compressed parallel to the direction of the hollow CaP filaments. In addition, the mechanical properties of porous CaP scaffolds could be tailored by adjusting their porosity, for example, compressive strengths of 4.8 ± 1.1 MPa at a porosity of ~82 vol %. The porous CaP scaffold showed good biocompatibility, which was assessed by in vitro cell tests, where several the cells adhered to and spread actively with the outer and inner surfaces of the hollow CaP filaments.

Bioactive Materials in Endodontics: An Evolving Component of Clinical Dentistry.

PubMed

Mohapatra, Satyajit; Patro, Swadheena; Mishra, Sumita

2016-06-01

Achieving biocompatibility in a material requires an interdisciplinary approach that involves a sound knowledge of materials science, bioengineering, and biotechnology. The host microbial-material response is also critical. Endodontic treatment is a delicate procedure that must be planned and executed properly. Despite major advances in endodontic therapy in recent decades, clinicians are confronted with a complex root canal anatomy and a wide selection of endodontic filling materials that, in turn, may not be well tolerated by the periapical tissues and may evoke an immune reaction. This article discusses published reports of various bioactive materials that are used in endodontic therapy, including calcium hydroxide, mineral trioxide aggregate, a bioactive dentin substrate, calcium phosphate ceramics, and calcium phosphate cements.

Method of coating a substrate with a calcium phosphate compound

DOEpatents

Gao, Yufei; Campbell, Allison A.

2000-01-01

The present invention is a method of coating a substrate with a calcium phosphate compound using plasma enhanced MOCVD. The substrate is a solid material that may be porous or non-porous, including but not limited to metal, ceramic, glass and combinations thereof. The coated substrate is preferably used as an implant, including but not limited to orthopaedic, dental and combinations thereof. Calcium phosphate compound includes but is not limited to tricalcium phosphate (TCP), hydroxyapatite (HA) and combinations thereof. TCP is preferred on a titanium implant when implant resorbability is desired. HA is preferred when the bone bonding of new bone tissue into the structure of the implant is desired. Either or both of TCP and/or HA coated implants may be placed into a solution with an agent selected from the group of protein, antibiotic, antimicrobial, growth factor and combinations thereof that can be adsorbed into the coating before implantation. Once implanted, the release of TCP will also release the agent to improve growth of new bone tissues and/or to prevent infection.

Biomimetic Coating on Porous Alumina for Tissue Engineering: Characterisation by Cell Culture and Confocal Microscopy

PubMed Central

Kolos, Elizabeth; Ruys, Andrew J

2015-01-01

In this study porous alumina samples were prepared and then coated using the biomimetic coating technique using a five times Simulated Body Fluid (5.0SBF) as the growth solution. A coating was achieved after pre-treatment with concentrated acid. From elemental analysis, the coating contained calcium and phosphorous, but also sodium and chlorine. Halite was identified by XRD, a sodium chloride phase. Sintering was done to remove the halite phase. Once halite was burnt off, the calcium phosphate crystals were not covered with halite and, therefore, the apatite phases can be clearly observed. Cell culturing showed sufficient cell attachment to the less porous alumina, Sample B, that has more calcium phosphate growth, while the porous alumina, Sample A, with minimal calcium phosphate growth attained very little cell attachment. This is likely due to the contribution that calcium phosphate plays in the attachment of bone-like cells to a bioinert ceramic such as alumina. These results were repeated on both SEM and confocal microscopy analysis. Confocal microscopy was a novel characterisation approach which gave useful information and was a visual aid.

Spark Plasma Sintering of Load-Bearing Iron-Carbon Nanotube-Tricalcium Phosphate CerMets for Orthopaedic Applications

NASA Astrophysics Data System (ADS)

Montufar, Edgar B.; Horynová, Miroslava; Casas-Luna, Mariano; Diaz-de-la-Torre, Sebastián; Celko, Ladislav; Klakurková, Lenka; Spotz, Zdenek; Diéguez-Trejo, Guillermo; Fohlerová, Zdenka; Dvorak, Karel; Zikmund, Tomáš; Kaiser, Jozef

2016-04-01

Recently, ceramic-metallic composite materials (CerMets) have been investigated for orthopaedic applications with promising results. This first generation of bio-CerMets combine the bioactivity of hydroxyapatite with the mechanical stability of titanium to fabricate bioactive, tough and biomechanically more biocompatible osteosynthetic devices. Nonetheless, these first CerMets are not biodegradable materials and a second surgery is required to remove the implant after bone healing. The present work aims to develop the next generation bio-CerMets, which are potential biodegradable materials. The process to produce the new biodegradable CerMet consisted of mixing powder of soluble and osteoconductive alpha tricalcium phosphate with biocompatible and biodegradable iron with consolidation through spark plasma sintering (SPS). The microstructure, composition and mechanical strength of the new CerMet were studied by metallography, x-ray diffraction and diametral tensile strength tests, respectively. The results show that SPS produces CerMet with higher mechanical performance (120 MPa) than the ceramic component alone (29 MPa) and similar mechanical strength to the pure metallic component (129 MPa). Nonetheless, although a short sintering time (10 min) was used, partial transformation of the alpha tricalcium phosphate into its allotropic and slightly less soluble beta phase was observed. Cell adhesion tests show that osteoblasts are able to attach to the CerMet surface, presenting spread morphology regardless of the component of the material with which they are in contact. However, the degradation process restricted to the small volume of the cell culture well quickly reduces the osteoblast viability.

Microgravity Science and Applications Program Tasks, 1984 Revision

NASA Technical Reports Server (NTRS)

Pentecost, E. (Compiler)

1985-01-01

This report is a compilation of the active research tasks as of the end of the fiscal year 1984 of the Microgravity Science and Applications Program, NASA-Office of Space Science and Applications, involving several NASA centers and other organizations. The purpose of the document is to provide an overview of the program scope for managers and scientists in industry, university, and government communities. The report is structured to include an introductory description of the program, strategy and overall goal; identification of the organizational structures and people involved; and a description of each research task, together with a list of recent publications. The tasks are grouped into six categories: (1) electronic materials; (2) solidification of metals, alloys, and composites; (3) fluid dynamics and transports; (4) biotechnology; (5) glasses and ceramics; and (6) combustion.

Microgravity Science and Application Program tasks, 1989 revision

NASA Technical Reports Server (NTRS)

1990-01-01

The active research tasks, as of the fiscal year 1989, of the Microgravity Science and Applications Program, NASA Office of Space Science and Applications, involving several NASA Centers and other organizations are compiled. The purpose is to provide an overview of the program scope for managers and scientists in industry, university, and government communities. The scientists in industry, university, and government communities. An introductory description of the program, the strategy and overall goal, identification of the organizational structures and people involved, and a description of each task are included. Also provided is a list of recent publications. The tasks are grouped into several major categories: electronic materials, solidification of metals, alloys, and composites; fluids, interfaces, and transport; biotechnology; glasses and ceramics; combustion science; physical and chemistry experiments (PACE); and experimental technology, facilities, and instrumentation.

Microgravity Science and Applications Program tasks, 1990 revision

NASA Technical Reports Server (NTRS)

1991-01-01

The active research tasks as of the end of the fiscal year 1990 sponsored by the Microgravity Science and Applications Division of the NASA Office of Space Science and Applications are compiled. The purpose is to provide an overview of the program scope for managers and scientists in industry, university, and government communities. The report includes an introductory description of the program, the strategy and overall goal; an index of principle investigators; and a description of each task. A list of recent publications is also provided. The tasks are grouped into six major categories: electronic materials; solidification of metals, alloys, and composites; fluid dynamics and transport phenomena; biotechnology; glasses and ceramics; combustion; experimental technology; facilities; and Physics And Chemistry Experiments (PACE). The tasks are divided into ground-based and flight experiments.

Microstructure and spectroscopic investigations of calcium zinc bismuth phosphate glass ceramics doped with manganese ions

NASA Astrophysics Data System (ADS)

Suneel Kumar, A.; Sambasiva Rao, M. V.; Chinna Ram, G.; Krishna Rao, D.

2018-01-01

Multi-component 10CaF2-20ZnO-(15 - x)Bi2O3-55P2O5:xMnO (0 ≤ x ≤ 2.5) glass ceramics were synthesised by melt quenching technique and heat treatment. The prepared glass ceramics were characterised by XRD, DTA, EDS and SEM. Spectroscopic studies such as optical absorption, EPR, FTIR and Raman were also carried out on these glass ceramics. The XRD and SEM studies have indicated that ceramic samples contain well defined and randomly distributed grains of different crystalline phases. The observed increase of enthalpy from DTA patterns up to 1 mol% of MnO indicates that the crystallisation starts initially from the surface of the material then gradually it is extended to the volume of the material and this influence is meagre at higher concentrations of MnO. The absorption spectra of manganese doped glass ceramics have exhibited two types of conventional bands; one due to Mn2+ ions and other due to Mn3+ ions. The EPR spectra of MnO doped glass ceramics showed a resonance signal around g2 = 2.023 with a six line hyperfine structure and another signal at about g1 = 4.314. The relative intensity and half-width of these two signals are observed to increase with the increase in the concentration of manganese ions up to 1 mol% beyond this concentration it is found to decrease. Such observation indicates the conversion of part of Mn2+ ions into Mn3+ ions in the glass ceramic matrix. The observed increase in the intensity of symmetrical structural units at the expense of asymmetrical structural units from the FTIR and Raman spectra at higher concentration of MnO indicating that Mn2+ ions occupy the network forming positions in the glass ceramic structure.

Advanced diesel engine component development program, tasks 4-14

NASA Astrophysics Data System (ADS)

Kaushal, Tony S.; Weber, Karen E.

1994-11-01

This report summarizes the Advanced Diesel Engine Component Development (ADECD) Program to develop and demonstrate critical technology needed to advance the heavy-duty low heat rejection engine concept. Major development activities reported are the design, analysis, and fabrication of monolithic ceramic components; vapor phase and solid film lubrication; electrohydraulic valve actuation; and high pressure common rail injection. An advanced single cylinder test bed was fabricated as a laboratory tool in studying these advanced technologies. This test bed simulates the reciprocator for a system having no cooling system, turbo compounding, Rankine bottoming cycle, common rail injection, and variable valve actuation to achieve fuel consumption of 160 g/kW-hr (.26 lb/hp-hr). The advanced concepts were successfully integrated into the test engine. All ceramic components met their functional and reliability requirements. The firedeck, cast-in-place ports, valves, valve guides, piston cap, and piston ring were made from silicon nitride. Breakthroughs required to implement a 'ceramic' engine included the fabrication of air-gap cylinder heads, elimination of compression gaskets, machining of ceramic valve seats within the ceramic firedeck, fabrication of cast-in-place ceramic port liners, implementation of vapor phase lubrication, and elimination of the engine coolant system. Silicon nitride valves were successfully developed to meet several production abuse test requirements and incorporated into the test bed with a ceramic valve guide and solid film lubrication. The ADECD cylinder head features ceramic port shields to increase insulation and exhaust energy recovery. The combustion chamber includes a ceramic firedeck and piston cap. The tribological challenge posed by top ring reversal temperatures of 550 C was met through the development of vapor phase lubrication using tricresyl phosphate at the ring-liner interface. A solenoid-controlled, variable valve actuation system that eliminated the conventional camshaft was demonstrated on the test bed. High pressure fuel injection via a common rail system was also developed to reduce particulate emissions.

Osteoblast and osteoclast responses to A/B type carbonate-substituted hydroxyapatite ceramics for bone regeneration.

PubMed

Germaini, Marie-Michèle; Detsch, Rainer; Grünewald, Alina; Magnaudeix, Amandine; Lalloue, Fabrice; Boccaccini, Aldo R; Champion, Eric

2017-06-06

The influence of carbonate substitution (4.4 wt%, mixed A/B type) in hydroxyapatite ceramics for bone remodeling scaffolds was investigated by separately analyzing the response of pre-osteoblasts and osteoclast-like cells. Carbonated hydroxyapatite (CHA) (Ca 9.5 (PO 4 ) 5.5 (CO 3 ) 0.5 (OH)(CO 3 ) 0.25 -CHA), mimicking the chemical composition of natural bone mineral, and pure hydroxyapatite (HA) (Ca 10 (PO 4 ) 6 (OH) 2 -HA) porous ceramics were processed to obtain a similar microstructure and surface physico-chemical properties (grain size, porosity ratio and pore size, surface roughness and zeta potential). The biological behavior was studied using MC3T3-E1 pre-osteoblastic and RAW 264.7 monocyte/macrophage cell lines. Chemical dissolution in the culture media and resorption lacunae produced by osteoclasts occur with both HA and CHA ceramics, but CHA exhibits much higher dissolution and greater bioresorption ability. CHA ceramics promoted a significantly higher level of pre-osteoblast proliferation. Osteoblastic differentiation, assessed by qRT-PCR of RUNX2 and COLIA2, and pre-osteoclastic proliferation and differentiation were not significantly different on CHA or HA ceramics but cell viability and metabolism were significantly greater on CHA ceramics. Thus, the activity of both osteoclast-like and osteoblastic cells was influenced by the carbonate substitution in the apatite structure. Furthermore, CHA showed a particularly interesting balance between biodegradation, by osteoclasts and chemical dissolution, and osteogenesis through osteoblasts' activity, to stimulate bone regeneration. It is hypothesized that this amount of 4.4 wt% carbonate substitution leads to an adapted concentration of calcium in the fluid surrounding the ceramic to stimulate the activity of cells. These results highlight the superior biological behavior of microporous 4.4 wt% A/B CHA ceramics that could beneficially replace the commonly used HA of biphasic calcium phosphates for future applications in bone tissue engineering.

In vitro evaluation of microleakage of various types of dental cements.

PubMed

Medić, Vesna; Obradović-Djuricić, Kosovka; Dodić, Slobodan; Petrović, Renata

2010-01-01

Microleakage is defined as the clinically undetectable seepage of oral fluids containing bacteria and debris between cement layer and tooth restoration. This in vitro study investigated the effect of different dental cements (zinc-phosphate, polycarboxylate, glass-ionomer and resin cement) on microleakage in different ceramic crown systems (metal ceramic crown, metal ceramic crown with a porcelain margin, Empress 2 and in Ceram all-ceramic crowns) fixed on extracted human teeth. One hundred and sixty intact human premolars were randomized to four groups of forty teeth each, according to the different ceramic crown systems. They were prepared in a standardized manner for metal-ceramic and all-ceramic crowns. Crowns were made following a standard laboratory technique, and each group of crowns were divided into four groups according to the different cement agents and cemented on their respective abutments. The specimens were subjected to thermocycling, placed in methylene blue solutions, embedded in resin blocks and vertically cut in the bucco-oral and meso-distal direction. The microleakage in the area of tooth-cement interface was defined as linear penetration of methylene blue and was determined with a microscope to assign microleakage scores using a five-point scale. A significant association was found between a cement type and degree of microleakage (p = 0.001). No statistically significant differences were found among the different ceramic crown systems luted with the same dental cement. The smallest degree of microleakage was observed in specimens luted with resin cement (X = 1.73), followed by glass-ionomer cement (X=2.45) and polycarboxylate cement (X = 3.20). The greatest degree of microleakage was detected in the crowns fixed with zincphosphate cement (X = 3.33). The investigated dental cements revealed different sealing abilities. The use of resin cement resulted in the percentage of 0 microleakage scores. Due to this feature, the resin cement is to be recommended in everyday clinical practice.

Advanced diesel engine component development program, tasks 4-14

NASA Technical Reports Server (NTRS)

Kaushal, Tony S.; Weber, Karen E.

1994-01-01

This report summarizes the Advanced Diesel Engine Component Development (ADECD) Program to develop and demonstrate critical technology needed to advance the heavy-duty low heat rejection engine concept. Major development activities reported are the design, analysis, and fabrication of monolithic ceramic components; vapor phase and solid film lubrication; electrohydraulic valve actuation; and high pressure common rail injection. An advanced single cylinder test bed was fabricated as a laboratory tool in studying these advanced technologies. This test bed simulates the reciprocator for a system having no cooling system, turbo compounding, Rankine bottoming cycle, common rail injection, and variable valve actuation to achieve fuel consumption of 160 g/kW-hr (.26 lb/hp-hr). The advanced concepts were successfully integrated into the test engine. All ceramic components met their functional and reliability requirements. The firedeck, cast-in-place ports, valves, valve guides, piston cap, and piston ring were made from silicon nitride. Breakthroughs required to implement a 'ceramic' engine included the fabrication of air-gap cylinder heads, elimination of compression gaskets, machining of ceramic valve seats within the ceramic firedeck, fabrication of cast-in-place ceramic port liners, implementation of vapor phase lubrication, and elimination of the engine coolant system. Silicon nitride valves were successfully developed to meet several production abuse test requirements and incorporated into the test bed with a ceramic valve guide and solid film lubrication. The ADECD cylinder head features ceramic port shields to increase insulation and exhaust energy recovery. The combustion chamber includes a ceramic firedeck and piston cap. The tribological challenge posed by top ring reversal temperatures of 550 C was met through the development of vapor phase lubrication using tricresyl phosphate at the ring-liner interface. A solenoid-controlled, variable valve actuation system that eliminated the conventional camshaft was demonstrated on the test bed. High pressure fuel injection via a common rail system was also developed to reduce particulate emissions.

Effect of the biodegradation rate controlled by pore structures in magnesium phosphate ceramic scaffolds on bone tissue regeneration in vivo.

PubMed

Kim, Ju-Ang; Lim, Jiwon; Naren, Raja; Yun, Hui-Suk; Park, Eui Kyun

2016-10-15

Similar to calcium phosphates, magnesium phosphate (MgP) ceramics have been shown to be biocompatible and support favorable conditions for bone cells. Micropores below 25μm (MgP25), between 25 and 53μm (MgP53), or no micropores (MgP0) were introduced into MgP scaffolds using different sizes of an NaCl template. The porosities of MgP25 and MgP53 were found to be higher than that of MgP0 because of their micro-sized pores. Both in vitro and in vivo analysis showed that MgP scaffolds with high porosity promoted rapid biodegradation. Implantation of the MgP0, MgP25, and MgP53 scaffolds into rabbit calvarial defects (with 4- and 6-mm diameters) was assessed at two times points (4 and 8weeks), followed by analysis of bone regeneration. The micro-CT and histologic analyses of the 4-mm defect showed that the MgP25 and MgP53 scaffolds were degraded completely at 4weeks with simultaneous bone and marrow-like structure regeneration. For the 6-mm defect, a similar pattern of regeneration was observed. These results indicate that the rate of degradation is associated with bone regeneration. The MgP25 and MgP53 scaffold-implanted bone showed a better lamellar structure and enhanced calcification compared to the MgP0 scaffold because of their porosity and degradation rate. Tartrate-resistant acid phosphatase (TRAP) staining indicated that the newly formed bone was undergoing maturation and remodeling. Overall, these data suggest that the pore architecture of MgP ceramic scaffolds greatly influence bone formation and remodeling activities and thus should be considered in the design of new scaffolds for long-term bone tissue regeneration. The pore structural conditions of scaffold, including porosity, pore size, pore morphology, and pore interconnectivity affect cell ingrowth, mechanical properties and biodegradabilities, which are key components of scaffold in bone tissue regeneration. In this study, we designed hierarchical pore structure of the magnesium phosphate (MgP) scaffold by combination of the 3D printing process, self-setting reaction and salt-leaching technique, and first studied the effect of pore structures of bioceramic scaffolds on bone tissue regeneration through both in vitro and in vivo studies (rabbit calvarial model). The MgP scaffolds with higher porosity promoted more rapid biodegradation and enhanced new bone formation and remodeling activities at the same time. Copyright © 2016 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Development of calcium phosphate cement using chitosan and citric acid for bone substitute materials.

PubMed

Yokoyama, Atsuro; Yamamoto, Satoru; Kawasaki, Takao; Kohgo, Takao; Nakasu, Masanori

2002-02-01

We developed a calcium phosphate cement that could be molded into any desired shape due to its chewing-gum-like consistency after mixing. The powder component of the cement consists of alpha-tricalcium phosphate and tetracalcium phosphate, which were made by decomposition of hydroxyapatite ceramic blocks. The liquid component consists of citric acid, chitosan and glucose solution. In this study, we used 20% citric acid (group 20) and 45% citric acid (group 45). The mechanical properties and biocompatibility of this new cement were investigated. The setting times of cements were 5.5 min, in group 20 and 6.4 min, in group 45. When incubated in physiological saline, the cements were transformed to hydroxyapatite at 3, and 6 weeks, the compressive strengths were 15.6 and 20.7 MPa, in group 45 and group 20, respectively. The inflammatory response around the cement implanted on the bone and in the subcutaneous tissue in rats was more prominent in group 45 than in group 20 at 1 week after surgery. After 4 weeks, the inflammation disappeared and the cement had bound to bone in both groups. These results indicate that this new calcium phosphate cement is a suitable bone substitute material and that the concentration of citric acid in the liquid component affects its mechanical properties and biocompatibility.

Studies on sintering additives for hydroxyapatite, and controlled porosity structures of calcium aluminates and polypropylene-tricalcium phosphate for bone graft applications

NASA Astrophysics Data System (ADS)

Kalita, Samar Jyoti

Tissue engineering has made a significant contribution in developing new biomaterials that can restore the structural features and physiological functions of natural tissues. Various materials, such as metals, ceramics, polymers and composites have been developed for their use in hard tissue engineering applications. Part A of this thesis describes my research on HAp ceramics. HAp, a bioactive ceramic, is known for its osteoconductivity, but shows poor mechanical performance. This program aimed at improving mechanical performance of synthetic HAp by introducing small quantities of various sintering additives. A range of oxide-based sintering additives were selected and prepared. Dense compacts were prepared using a uniaxial press with an average green density of 1.6 g/cc. Results showed that some of these sintering additives improved densification, hardness and compression strength of synthetic HAp compared to the pure composition. A maximum bulk density of 3.06 g/cc was achieved for 2.5 wt% addition of MgO. A Microhardness of 4.9 GPa (505 HV) was measured for 2.5 wt% addition of BaO, and the highest compression strength (220MPa) was reported for 2.5 wt% addition of CaO. Cytotoxicity and cell proliferation studies with a modified human osteoblast (HOB) cell-line (OPC1) proved most of these materials non-toxic and biocompatible. Microscopic observation revealed that bone cells were attached and grew well on most of these ceramic matrices. Part B describes my work on development of controlled porosity polypropylene-tricalcium phosphate composite scaffolds via the fused deposition modeling (FDM) process. Hg-porosimetry was performed to determine pore size and their distribution. Uniaxial compression testing performed on samples with 36 vol% porosity and pore size of 160 mum showed the best compressive strength of 12.7 MPa. Part C includes my research on development of "3-D honeycomb" porous calcium aluminate structures via the indirect FDM process. Samples of 29% and 44% VFP (designed) with average pore size of 300 mum showed compressive strength between 2 and 24 MPa. Cell proliferation studies conducted with OPC1 cells on polymer-ceramic composite scaffolds and porous calcium aluminate structures showed good cell attachment and a steady cell growth behavior during the first three weeks of in vitro analyses.

Advantageous new conic cannula for spine cement injection.

PubMed

González, Sergio Gómez; Vlad, María Daniela; López, José López; Aguado, Enrique Fernández

2014-09-01

Experimental study to characterize the influence of the cannula geometry on both, the pressure drop and the cement flow velocity established along the cannula. To investigate how the new experimental geometry of cannulas can affect the extravertebral injection pressure and the velocity profiles established along the cannula during the injection process. Vertebroplasty procedure is being used to treat vertebral compression fractures. Vertebra infiltration is favored by the use of suitable: (1) syringes or injector devices; (2) polymer or ceramic bone cements; and (3) cannulas. However, the clinical use of ceramic bone cement has been limited due to press-filtering problems. Thus, new approaches concerning the cannula geometry are needed to minimize the press-filtering of calcium phosphate-based bone cements and thereby broaden its possible applications. Straight, conic, and combined conic-straight new cannulas with different proximal and distal both length and diameter ratios were drawn with computer-assisted design software. The new geometries were theoretically analyzed by: (1) Hagen-Poisseuille law; and (2) computational fluid dynamics. Some experimental models were manufactured and tested for extrusion in order to confirm and further advance the theoretical results. The results confirm that the totally conic cannula model, having proximal to distal diameter ratio equal 2, requires the lowest injection pressure. Furthermore, its velocity profile showed no discontinuity at all along the cannula length, compared with other known combined proximal and distal straight cannulas, where discontinuity was produced at the proximal-distal transition zone. The conclusion is that the conic cannulas: (a) further reduced the extravertebral pressure during the injection process; (b) showed optimum fluid flow velocity profiles to minimize filter-pressing problems, especially when ceramic cements are used; and (c) can be easily manufactured. In this sense, the new conic cannulas should favor the use of calcium phosphate bone cements in the spine. N/A.

Influence of surface porosity and pH on bacterial adherence to hydroxyapatite and biphasic calcium phosphate bioceramics.

PubMed

Kinnari, Teemu J; Esteban, Jaime; Martin-de-Hijas, Nieves Z; Sánchez-Muñoz, Orlando; Sánchez-Salcedo, Sandra; Colilla, Montserrat; Vallet-Regí, María; Gomez-Barrena, Enrique

2009-01-01

Hydroxyapatite (HA) and biphasic calcium phosphate (BCP) ceramic materials are widely employed as bone substitutes due to their porous and osteoconductive structure. Their porosity and the lowering of surrounding pH as a result of surgical trauma may, however, predispose these materials to bacterial infections. For this reason, the influence of porosity and pH on the adherence of common Gram-positive bacteria to the surfaces of these materials requires investigation. Mercury intrusion porosimetry measurements revealed that the pore size distribution of both bioceramics had, on a logarithmic scale, a sinusoidal frequency distribution ranging from 50 to 300 nm, with a mean pore diameter of 200 nm. Moreover, total porosity was 20 % for HA and 50 % for BCP. Adherence of Staphylococcus aureus and Staphylococcus epidermidis was studied at a physiological pH of 7.4 and at a pH simulating bone infection of 6.8. Moreover, the effect of pH on the zeta potential of HA, BCP and of both staphylococci was evaluated. Results showed that when pH decreased from 7.4 to 6.8, the adherence of both staphylococci to HA and BCP surfaces decreased significantly, although at the same time the negative zeta-potential values of the ceramic surfaces and both bacteria diminished. At both pH values, the number of S. aureus adhered to the HA surface appeared to be lower than that for BCP. A decrease in pH to 6.8 reduced the adherence of both bacterial species (mean 57 %). This study provides evidence that HA and BCP ceramics do not have pores sufficiently large to allow the internalization of staphylococci. Their anti-adherent properties seemed to improve when pH value decreased, suggesting that HA and BCP bioceramics are not compromised upon orthopaedic use.

Development of Bioactive Ceramic Coating on Titanium Alloy substrate for Biomedical Application Using Dip Coating Method

NASA Astrophysics Data System (ADS)

Asmawi, R.; Ibrahim, M. H. I.; Amin, A. M.; Mustafa, N.; Noranai, Z.

2017-08-01

Bioactive apatite, such as hydroxyapatite ceramic (HA), [Ca10(PO4)6(OH)2] has been extensively investigated for biomedical applications due to its excellent biocompatibility and tissue bioactivity properties. Its bioactivity provides direct bonding to the bone tissue. Because of its similarity in chemical composition to the inorganic matrix of bone, HA is widely used as implant materials for bone. Unfortunately, because of its poor mechanical properties,. this bioactive material is not suitable for load bearing applications. In this study, by the assistance of dip-coating technique, HA coatings were deposited on titanium alloy substrates by employing hydrothermal derived HA powder. The produced coatings then were oven-dried at 130°C for 1 hour and calcined at various temperature over the range of 200-800°C for 1 hour. XRD measurement showed that HA was the only phase present in the coatings. However coatings calcined at 800°C comprised a mixture of HA and tri-calcium phosphate (TCP). FTIR measurement showed the existence of hydroxyl, phosphate, and carbonate bands. PO4 - band became sharper and narrower with the increased of calcination temperature. FESEM observation showed that the coating is polycrystalline with individual particles of nano to submicron size and has an average particle size of 35 nm. The thickness of the coating are direcly propotional with the viscosity of coating slurry. It was shown that the more viscous coating slurry would produce a thicker ceramic coating. Mechanical properties of the coating were measured in term of adhesion strength using a Micro Materials Nano Test microscratch testing machine. The result revealed that the coating had a good adhesion to the titanium alloy substrate.

Ageing of a phosphate ceramic used to immobilize chloride contaminated actinide waste

NASA Astrophysics Data System (ADS)

Metcalfe, B. L.; Donald, I. W.; Fong, S. K.; Gerrard, L. A.; Strachan, D. M.; Scheele, R. D.

2009-03-01

A process for the immobilization of intermediate level waste containing a significant quantity of chloride using Ca3(PO4)2 as the host material has been developed. Waste ions are incorporated into two phosphate-based phases, chlorapatite [Ca5(PO4)3Cl] and spodiosite [Ca2(PO4)Cl]. Non-active trials performed using Sm as the actinide surrogate demonstrated the durability of these phases in aqueous solution. Trials of the process, in which actinide-doped materials were used, were performed at PNNL which confirmed the wasteform resistant to aqueous leaching. Initial leach trials conducted on 239Pu/241Am loaded ceramic at 313 K/28 days gave normalized mass losses of 1.2 × 10-5 g m-2 and 2.7 × 10-3 g m-2 for Pu and Cl, respectively. In order to assess the response of the phases to radiation-induced damage, accelerated ageing trials were performed on samples in which the 239Pu was replaced with 238Pu. No changes to the crystalline structure of the waste were detected in the XRD spectra after the samples had experienced an α radiation fluence of 4 × 1018 g-1. Leach trials showed that there was an increase in the P and Ca release rates but no change in the Pu release rate.

Microstereolithography-Based Fabrication of Anatomically Shaped Beta-Tricalcium Phosphate Scaffolds for Bone Tissue Engineering

PubMed Central

Du, Dajiang; Asaoka, Teruo; Shinohara, Makoto; Kageyama, Tomonori; Ushida, Takashi; Furukawa, Katsuko Sakai

2015-01-01

Porous ceramic scaffolds with shapes matching the bone defects may result in more efficient grafting and healing than the ones with simple geometries. Using computer-assisted microstereolithography (MSTL), we have developed a novel gelcasting indirect MSTL technology and successfully fabricated two scaffolds according to CT images of rabbit femur. Negative resin molds with outer 3D dimensions conforming to the femur and an internal structure consisting of stacked meshes with uniform interconnecting struts, 0.5 mm in diameter, were fabricated by MSTL. The second mold type was designed for cortical bone formation. A ceramic slurry of beta-tricalcium phosphate (β-TCP) with room temperature vulcanization (RTV) silicone as binder was cast into the molds. After the RTV silicone was completely cured, the composite was sintered at 1500°C for 5 h. Both gross anatomical shape and the interpenetrating internal network were preserved after sintering. Even cortical structure could be introduced into the customized scaffolds, which resulted in enhanced strength. Biocompatibility was confirmed by vital staining of rabbit bone marrow mesenchymal stromal cells cultured on the customized scaffolds for 5 days. This fabrication method could be useful for constructing bone substitutes specifically designed according to local anatomical defects. PMID:26504839

Nanostructured bioactive glass-ceramic coatings deposited by the liquid precursor plasma spraying process

NASA Astrophysics Data System (ADS)

Xiao, Yanfeng; Song, Lei; Liu, Xiaoguang; Huang, Yi; Huang, Tao; Wu, Yao; Chen, Jiyong; Wu, Fang

2011-01-01

Bioactive glass-ceramic coatings have great potential in dental and orthopedic medical implant applications, due to its excellent bioactivity, biocompatibility and osteoinductivity. However, most of the coating preparation techniques either produce only thin thickness coatings or require tedious preparation steps. In this study, a new attempt was made to deposit bioactive glass-ceramic coatings on titanium substrates by the liquid precursor plasma spraying (LPPS) process. Tetraethyl orthosilicate, triethyl phosphate, calcium nitrate and sodium nitrate solutions were mixed together to form a suspension after hydrolysis, and the liquid suspension was used as the feedstock for plasma spraying of P 2O 5-Na 2O-CaO-SiO 2 bioactive glass-ceramic coatings. The in vitro bioactivities of the as-deposited coatings were evaluated by soaking the samples in simulated body fluid (SBF) for 4 h, 1, 2, 4, 7, 14, and 21 days, respectively. The as-deposited coating and its microstructure evolution behavior under SBF soaking were systematically analyzed by scanning electron microscopy (SEM), X-ray diffraction (XRD), inductively coupled plasma (ICP), and Fourier transform infrared (FTIR) spectroscopy. The results showed that P 2O 5-Na 2O-CaO-SiO 2 bioactive glass-ceramic coatings with nanostructure had been successfully synthesized by the LPPS technique and the synthesized coatings showed quick formation of a nanostructured HCA layer after being soaked in SBF. Overall, our results indicate that the LPPS process is an effective and simple method to synthesize nanostructured bioactive glass-ceramic coatings with good in vitro bioactivity.

Influence of contamination on bonding to zirconia ceramic.

PubMed

Yang, Bin; Scharnberg, Michael; Wolfart, Stefan; Quaas, Anne C; Ludwig, Klaus; Adelung, Rainer; Kern, Matthias

2007-05-01

The purpose of this study was to investigate the influences of contaminations and cleaning methods on bonding to dental zirconia ceramic. After saliva immersion and using silicone disclosing agent, airborne-particle abraded ceramic specimens were cleaned with isopropanol (AL), acetone (AC), 37% phosphoric acid (PA), additional airborne-particle abrasion (AA), or only with water rinsing (SS). Airborne-particle abraded specimens without contaminations (CL) were used as control group. For chemical analysis specimens of all groups were examined with X-ray photoelectron spectroscopy (XPS). Plexiglas tubes filled with composite resin were bonded to ceramic specimens using a phosphate-monomer containing composite luting resin. After 3-day water storage, tensile bond strengths (TBS) were tested. XPS analysis of group SS showed the presence of saliva and silicone (Si) contamination on the surface. The ratios of carbon/zirconium and oxygen/zirconium for groups PA and AA were comparable to those ratios obtained for group CL, indicating the removal of the organic saliva contamination. Airborne-particle abrasion and acetone completely removed Si contamination from ceramic surfaces. Isopropanol had little cleaning effect on the two contaminants. TBS (median +/- standard deviation) in MPa of the groups SS (11.6 +/- 3.1), AL (10.0 +/- 2.9), and AC (13.0 +/- 2.8) were statistically lower than those of groups PA (33.6 +/- 5.5), AA (40.1 +/- 3.6), and CL (47.0 +/- 8.1) (p < 0.001), while no differences were found in TBS between groups AA and CL (p > 0.5). Contamination significantly reduced bond strengths to zirconia ceramic. Airborne-particle abrasion was the most effective cleaning method.

Fabrication of Rare-earth Aluminate (ReAlO3) Glass and Crystalline phases by Aerodynamic Levitation (ADL)

NASA Astrophysics Data System (ADS)

Basavalingu, B.; Yoda, Shinichi; Kumar, M. S. Vijaya

2012-07-01

Containerless processing by levitation technique has been extensively used for material science and engineering because it suppresses inhomogeneous nucleation from the container wall and helps to produce stable, metastable and glass phases. The containerless levitation technique is widely explored for material processing because of its technological and scientific advantages. Recently, research on bulk glass and glass-ceramics have attracted the attention of material scientists as they are considered as low cost optical materials of the future. In the present study, the formation of bulk spherical glass and crystalline ReAlO _{3}(Re=La-Lu,Y) phases has been investigated due to their unique features in terms of the solidification process from an undercooled melt, glass structure and optical properties. An Aerodynamic levitation (ADL) was used to undercool the melt well below the melting temperature. Sintered bits of ReAlO _{3} sample with a diameter of ~2.5 mm and mass of ~20-25 mg was levitated by an ADL and completely melted by a CO _{2} laser and then the droplet was cooled by turning off the CO _{2} laser and solidified. The surface temperature and solidification process of the levitated droplet was monitored using pyrometer and high speed video camera, respectively. Among the rare earth aluminum perovskites Lanthanum, Neodymium and samarium aluminum perovskites solidified as glass and others YAlO _{3} and Europium to Lutetium aluminum perovskites solidified as crystalline phases. The scanning electron microscopy (SEM) images of cross-sectioned samples, TG/DTA, Transmittance and Refractive Index studies were performed for both glass and crystalline phases. The results of the above studies revealed the formation of glass and crystalline phases directly from the undercooled melt. The glass transition temperature (Tg) gradually increased with increasing ionic radius of the rare-earth elements. The NdAlO _{3} glass phase showed a high refractive index of ~1.89, suggesting that containerless levitation is an elegant technique for fabrication of new glass and crystalline ceramics from an undercooled melt.

Evaluation of calcination temperature and phase composition ratio for new hyroxyapatite

NASA Astrophysics Data System (ADS)

Salimi, M. N. Ahmad; Chin, H. S.

2017-10-01

The demand of production of hydroxyapatite (HA) has been increasing for the purpose of medical and dental application. HA possesses the excellent properties leads to the priority choice for ceramic bone replacement. Synthesis route by wet chemical precipitation is commonly practised in industrial scale. Calcium hydroxide and Orthophosphoric acid are the precursors for production scale. The synthesis of HA is conducted by varying the synthetic condition: stirring rate, calcium-phosphate and calcination temperature. This paper is focused on the properties of HA produced by regulating the synthetic condition so that the qualities of HA can be well performed. Characterization studies were also carried out by Fourier Transform Infrared Spectroscopy (FT-IR) for functional group identification, Scanning Electron Microscope (SEM) for surface morphology analysis and X-Ray Diffraction (XRD) for phase composition and crystallinity respectively. Narrow particle size distribution contributed to better quality of hydroxyapatite for bone replacement. Both calcium-phosphate ratio and calcination temperature would affect the phase composition of calcium phosphate.

Kinetic study of bone ingrowth and ceramic resorption associated with the implantation of different injectable calcium-phosphate bone substitutes.

PubMed

Gauthier, O; Bouler, J M; Weiss, P; Bosco, J; Daculsi, G; Aguado, E

1999-10-01

This study investigated the in vivo performance of two composite injectable bone substitutes (IBS), each with different calcium-phosphate particles granulometries [40-80 (IBS 40-80) and 200-500 microm (IBS 200-500)]. These biomaterials were obtained by associating a biphasic calcium-phosphate (BCP) ceramic mineral phase with a 3% aqueous solution of a cellulosic polymer (hydroxy-propyl-methyl-cellulose). Both materials were injected for periods of 2, 3, 8, or 12 weeks into bone defects at the distal end of rabbit femurs. Quantitative results on new bone formation, BCP resorption, and staining for tartrate-resistant acid phosphatase (TRAP) activity were studied for statistical purposes. Measurements with scanning electron microscopy and image analysis showed that the final rates of newly formed bone were similar for both tested IBS after 12 weeks of implantation. Bone colonization occurred more extensively during early implantation times for IBS 40-80 than for IBS 200-500. For the latter, BCP degradation occurred regularly throughout the implantation period, whereas it was very intensive during the first 2 weeks for IBS 40-80. Positive TRAP-stained degradation cells were significantly more numerous for IBS 40-80 than for IBS 200-500 regardless of implantation time. With the granulometry of either mineral phase, both tested IBS supported extensive bone colonization, which was greater than that previously reported for an equivalent block of macroporous BCP. The resorption-bone substitution process seemed to occur earlier and faster for IBS 40-80 than for IBS 200-500. Both tested IBS expressed similar biological efficiency, with conserved in vivo bioactivity and bone-filling ability. Copyright 1999 John Wiley & Sons, Inc.

Fabrication of individual alginate-TCP scaffolds for bone tissue engineering by means of powder printing.

PubMed

Castilho, Miguel; Rodrigues, Jorge; Pires, Inês; Gouveia, Barbara; Pereira, Manuel; Moseke, Claus; Groll, Jürgen; Ewald, Andrea; Vorndran, Elke

2015-01-06

The development of polymer-calcium phosphate composite scaffolds with tailored architectures and properties has great potential for bone regeneration. Herein, we aimed to improve the functional performance of brittle ceramic scaffolds by developing a promising biopolymer-ceramic network. For this purpose, two strategies, namely, direct printing of a powder composition consisting of a 60:40 mixture of α/β-tricalcium phosphate (TCP) powder and alginate powder or vacuum infiltration of printed TCP scaffolds with an alginate solution, were tracked. Results of structural characterization revealed that the scaffolds printed with 2.5 wt% alginate-modified TCP powders presented a uniformly distributed and interfusing alginate TCP network. Mechanical results indicated a significant increase in strength, energy to failure and reliability of powder-modified scaffolds with an alginate content in the educts of 2.5 wt% when compared to pure TCP, as well as to TCP scaffolds containing 5 wt% or 7.5 wt% in the educts, in both dry and wet states. Culture of human osteoblast cells on these scaffolds also demonstrated a great improvement of cell proliferation and cell viability. While in the case of powder-mixed alginate TCP scaffolds, isolated alginate gels were formed between the calcium phosphate crystals, the vacuum-infiltration strategy resulted in the covering of the surface and internal pores of the TCP scaffold with a thin alginate film. Furthermore, the prediction of the scaffolds' critical fracture conditions under more complex stress states by the applied Mohr fracture criterion confirmed the potential of the powder-modified scaffolds with 2.5 wt% alginate in the educts as structural biomaterial for bone tissue engineering.

Fabrication of β-tricalcium phosphate composite ceramic sphere-based scaffolds with hierarchical pore structure for bone regeneration.

PubMed

He, Fupo; Qian, Guowen; Ren, Weiwei; Li, Jiyan; Fan, Peirong; Shi, Haishan; Shi, Xuetao; Deng, Xin; Wu, Shanghua; Ye, Jiandong

2017-04-24

Polymer sphere-based scaffolds, which are prepared by bonding the adjacent spheres via sintering the randomly packed spheres, feature uniform pore structure, full three-dimensional (3D) interconnection, and considerable mechanical strength. However, bioceramic sphere-based scaffolds fabricated by this method have never been reported. Due to high melting temperature of bioceramic, only limited diffusion rate can be achieved when sintering the bioceramic spheres, which is far from enough to form robust bonding between spheres. In the present study, for the first time we fabricated 3D interconnected β-tricalcium phosphate ceramic sphere-based (PG/TCP) scaffolds by introducing phosphate-based glass (PG) as sintering additive and placing uniaxial pressure during the sintering process. The sintering mechanism of PG/TCP scaffolds was unveiled. The PG/TCP scaffolds had hierarchical pore structure, which was composed by interconnected macropores (>200 μm) among spheres, pores (20–120 μm) in the interior of spheres, and micropores (1–3 μm) among the grains. During the sintering process, partial PG reacted with β-TCP, forming β-Ca2P2O7; metal ions from PG substituted to Ca2+ sites of β-TCP. The mechanical properties (compressive strength 2.8–10.6 MPa; compressive modulus 190–620 MPa) and porosity (30%–50%) of scaffolds could be tailored by manipulating the sintering temperatures. The introduction of PG accelerated in vitro degradation of scaffolds, and the PG/TCP scaffolds showed good cytocompatibility. This work may offer a new strategy to prepare bioceramic scaffolds with satisfactory physicochemical properties for application in bone regeneration.

Comparative evaluation of different calcium phosphate-based bone graft granules - an in vitro study with osteoblast-like cells.

PubMed

Bernhardt, Anne; Lode, Anja; Peters, Fabian; Gelinsky, Michael

2013-04-01

Granule-shaped calcium phosphate-based bone graft materials are often required for bone regeneration especially in implant dentistry. Two newly developed bone graft materials are Ceracell(®) , an open-celled highly porous bioceramic from β-tricalcium phosphate (β-TCP) under addition of bioglass and Osseolive(®) , an open porous glass ceramic with the general formula Ca2 KNa(PO4 )2 . The goal of this study was to characterize different modifications of the two bone graft materials in vitro in comparison to already established ceramic bone grafts Cerasorb M(®) , NanoBone(®) and BONIT Matrix(®) . Adhesion and proliferation of SaOS-2 osteoblast-like cells were evaluated quantitatively by determining DNA content and lactate dehydrogenase (LDH) activity and qualitatively by scanning electron microscopy (SEM). In addition, MTT cell-vitality staining was applied to confirm the attachment of viable cells to the different materials. Osteogenic differentiation was evaluated by measurement of alkaline phosphatase (ALP) activity as well as gene expression analysis of osteogenic markers using reverse transcriptase PCR. DNA content and LDH activity revealed good cell attachment and proliferation for Ceracell and Cerasorb M. When pre-incubated with cell-culture medium, also Osseolive showed good cell attachment and proliferation. Attachment and proliferation of osteoblast-like cells on NanoBone and BONIT Matrix was very low, even after pre-incubation with cell-culture medium. Specific ALP activity on Ceracell(®) , Osseolive (®) and Cerasorb M(®) increased with time and expression of bone-related genes ALP, osteonectin, osteopontin and bone sialoprotein II was demonstrated. Ceracell as well as Osseolive granules support proliferation and osteogenic differentiation in vitro and may be promising candidates for in vivo applications. © 2011 John Wiley & Sons A/S.

Atomically resolved calcium phosphate coating on a gold substrate.

PubMed

Metoki, Noah; Baik, Sung-Il; Isheim, Dieter; Mandler, Daniel; Seidman, David N; Eliaz, Noam

2018-05-10

Some articles have revealed that the electrodeposition of calcium phosphate (CaP) coatings entails a precursor phase, similarly to biomineralization in vivo. The chemical composition of the initial layer and its thickness are, however, still arguable, to the best of our knowledge. Moreover, while CaP and electrodeposition of metal coatings have been studied utilizing atom-probe tomography (APT), the electrodeposition of CaP ceramics has not been heretofore studied. Herein, we present an investigation of the CaP deposition on a gold substrate. Using APT and transmission electron microscopy (TEM) it is found that a mixture of phases, which could serve as transient precursor phases to hydroxyapatite (HAp), can be detected. The thickness of these phases is tens of nanometers, and they consist of amorphous CaP (ACP), dibasic calcium phosphate dihydrate (DCPD), and octacalcium phosphate (OCP). This demonstrates the value of using atomic-resolved characterization techniques for identifying the precursor phases. It also indicates that the kinetics of their transformation into the more stable HAp is not too fast to enable their observation. The coating gradually displays higher Ca/P atomic ratios, a porous nature, and concomitantly a change in its density.

Synthesis of hollow spherical calcium phosphate nanoparticles using polymeric nanotemplates

NASA Astrophysics Data System (ADS)

Tjandra, Wiliana; Ravi, Palaniswamy; Yao, Jia; Tam, Kam C.

2006-12-01

Poly(methylmethacrylate)-block-poly(methacrylic acid) (PMMA-b-PMAA) copolymer was synthesized by an atom transfer radical polymerization (ATRP) technique. The block copolymer was employed as a template for the controlled precipitation of calcium phosphate from aqueous solution at different pH values. A Ca2+ ion selective electrode was used to study the interactions between Ca2+ ions and the polymer, which indicated a possible weak interaction between Ca2+ and un-ionized MAA segments at pH~4.0 in addition to electrostatic interaction between Ca2+ and ionized MAA segments at higher pH. An interesting structure representing that of a superstructure consisting of hybrid nano-filaments was observed by the transmission electron microscope at pH~4.0. The filaments originated from a core of similar size to primary polymer aggregates, suggesting that cooperative interactions at a local level between dissolving calcium phosphate clusters and disassembling polymer segments are responsible for the secondary growth process. A hollow spherical morphology was obtained at pH~7.0 and 9.0. Such calcium phosphate/polymer monohybrids with complex morphologies are interesting and might be useful as novel drug delivery carriers, ceramics precursors, reinforcing fillers or biomedical implants.

[Comparative study of bond strength between zirconia ceramics and 4 luting cements].

PubMed

Zheng, Hu; Zhang, Xian-Fang; Han, Dong-Wei

2007-02-01

To study the bonding strength of zirconia ceramics with 4 kinds of luting cement materials. Blocks of sintered zirconia ceramics were cut and randomly divided into 4 groups with 16 slices in each group. They were treated with sandblasting and bonded with 4 kinds of luting cements respectively. After preserved in 37 degrees C distilled-water for 24 hours and 30 days, the shear bonding strength of these specimens was tested and the data were analyzed by SAS6.12 software package and bond section were observed by scanning electron microscope. Two-way ANOVA revealed that the group of PanaviaF could attain the highest shear bonding strength: (34.7+/-3.44) MPa (after 24 hours), (31.5+/-3.44) MPa (after 1 month), which was significantly different from other treatment methods (P<0.01). The initial shear bonding strength of the groups of resin-reinforced glass ionomer was (15.5+/-2.71) MPa, (16.0+/-1.77) MPa (after 24 hours) but dropped markedly to (6.80+/-1.24) MPa, (3.38+/-2.32) MPa after 30 days (P<0.05). Resin luting cement containing phosphate monomer (MDP) can provide zirconia ceramics a strong and long-lasting bonding. Resin-reinforced glass ionomer can get good bonding strength too, but can't last long.

Microstructural Improvement of Hydroxyapatite-ZrO2 Composite Ceramics via Thermal Precipitation Techniques.

NASA Astrophysics Data System (ADS)

Sangmala, A.; Limsuwan, P.; Kaewwiset, W.; Naemchanthara, K.

2017-09-01

Hydroxyapatite-ZrO2 composite ceramic were synthesized using a thermal precipitation techniques. The chemical precursors were prepared from di-ammonium hydrogen orthophosphate, calcium oxide (CaO) derived from chicken eggshell, zirconium dioxide (ZrO2) and distilled water. The mixture were heated at the various temperatures from 100 to 700 °C in the furnace with an incremental temperature of 100 °C. The ZrO2 contents in the composite ceramic were varied from 0 to 15 percent weight of CaO. The prepared composites were then annealed at 300, 600 and 700 °C for 4 h in air. The crystal structure, function group and morphology of all samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), field emission scanning electron microscopy (FESEM) and universal testing machine (UTM), respectively. The results indicated that the undoped-ZrO2 samples hydroxyapatite phase with a hexagonal structure. However, the hydroxyapatite was transformed to the tri-calcium phosphate after thermal treatment at 700 °C. For the doped-ZrO2 samples, the hydroxyapatite and ZrO2 phases were found. Moreover, the result showed that the compressive strength of hydroxyapatite-ZrO2 composite ceramic increased with increasing the ZrO2 content.

Directionally solidified Al2O3/GAP eutectic ceramics by micro-pulling-down method

NASA Astrophysics Data System (ADS)

Cao, Xue; Su, Haijun; Guo, Fengwei; Tan, Xi; Cao, Lamei

2016-11-01

We reported a novel route to prepare directionally solidified (DS) Al2O3/GAP eutectic ceramics by micro-pulling-down (μ-PD) method. The eutectic crystallizations, microstructure characters and evolutions, and their mechanical properties were investigated in detail. The results showed that the Al2O3/GAP eutectic composites can be successfully fabricated through μ-PD method, possessed smooth surface, full density and large crystal size (the maximal size: φ90 mm × 20 mm). At the process of Diameter, the as-solidified Al2O3/GAP eutectic presented a combination of "Chinese script" and elongated colony microstructure with complex regular structure. Inside the colonies, the rod-type or lamellar-type eutectic microstructures with ultra-fine GAP surrounded by the Al2O3 matrix were observed. At an appropriate solidificational rate, the binary eutectic exhibited a typical DS irregular eutectic structure of "chinese script" consisting of interpenetrating network of α-Al2O3 and GAP phases without any other phases. Therefore, the interphase spacing was refined to 1-2 µm and the irregular microstructure led to an outstanding vickers hardness of 17.04 GPa and fracture toughness of 6.3 MPa × m1/2 at room temperature.

The directional crystallization of W-B-C- d-transition metal alloys

NASA Astrophysics Data System (ADS)

Paderno, Yuriy; Paderno, Varvara; Liashchenko, Alfred; Filipov, Volodymyr; Evdokimova, Alina; Martynenko, Anna

2006-09-01

Crystallization from the melt during arc melting and directional solidification during induction zone melting of pseudo-alloys tungsten carbide (WC)- MeB 2 ( Me—Ti, Zr, Cr) and a number of alloys of the W-B-C system (WB 0.12C 0.74; WB 0.25C 0.75; WB 0.34C 0.32; WB 0.49C 0.76; WB 0.59C 0.76; WB 0.89C 0.75; (WC) 0.9B 0.1) has been studied. It was shown that the alloys WC—80 mass%-ZrB 2—20 mass% and WC—72 mass%-WB—28 mass% are the closest ones to eutectic compositions. Investigation of the microstructure of eutectic alloys in the WC-WB system by thin foil method has revealed that both matrix and reinforcing phases are single crystalline. Hardness tests by indentation of the eutectic structure area ( P=10.3 N) do not result in radial crack formation, which is evidence of the essential plasticity of the obtained composite material. It is established that new ceramic-ceramic eutectic composite materials based on WC with transition metal diborides and with a boride phase of tungsten may be created. Such materials can be successfully applied in contemporary high-temperature techniques.

Bioactivity and cytotoxicity of glass and glass-ceramics based on the 3CaO·P₂O₅--SiO₂--MgO system.

PubMed

Daguano, Juliana K M F; Rogero, Sizue O; Crovace, Murilo C; Peitl, Oscar; Strecker, Kurt; Dos Santos, Claudinei

2013-09-01

The mechanical strength of bioactive glasses can be improved by controlled crystallization, turning its use as bulk bone implants viable. However, crystallization may affect the bioactivity of the material. The aim of this study was to develop glass-ceramics of the nominal composition (wt%) 52.75(3CaO·P₂O₅)-30SiO₂-17.25MgO, with different crystallized fractions and to evaluate their in vitro cytotoxicity and bioactivity. Specimens were heat-treated at 700, 775 and 975 °C, for 4 h. The major crystalline phase identified was whitlockite, an Mg-substituted tricalcium phosphate. The evaluation of the cytotoxicity was carried out by the neutral red uptake methodology. Ionic exchanges with the simulated body fluid SBF-K9 acellular solution during the in vitro bioactivity tests highlight the differences in terms of chemical reactivity between the glass and the glass-ceramics. The effect of crystallinity on the rates of hydroxycarbonate apatite (HCA) formation was followed by Fourier transformed infrared spectroscopy. Although all glass-ceramics can be considered bioactive, the glass-ceramic heat-treated at 775 °C (V775-4) presented the most interesting result, because the onset for HCA formation is at about 24 h and after 7 days the HCA layer dominates completely the spectrum. This occurs probably due to the presence of the whitlockite phase (3(Ca,Mg)O·P₂O₅). All samples were considered not cytotoxic.

Cellular compatibility of highly degradable bioactive ceramics for coating of metal implants.

PubMed

Radetzki, F; Wohlrab, D; Zeh, A; Delank, K S; Mendel, T; Berger, G; Syrowatka, F; Mayr, O; Bernstein, A

2011-01-01

Resorbable ceramics can promote the bony integration of implants. Their rate of degradation should ideally be synchronized with bone regeneration. This study examined the effect of rapidly resorbable calcium phosphate ceramics 602020, GB14, 305020 on adherence, proliferation and morphology of human bone-derived cells (HBDC) in comparison to β-TCP. The in vitro cytotoxicity was determined by the microculture tetrazolium (MTT) assay. HBDC were grown on the materials for 3, 7, 11, 15 and 19 days and counted. Cell morphology, cell attachment, cell spreading and the cytoskeletal organization of HBDC cultivated on the substrates were investigated using laser scanning microscopy and environmental scanning electron microscopy. All substrates supported sufficient cellular growth for 19 days and showed no cytotoxicity. On each material an identical cell colonisation of well communicating, polygonal, vital cells with strong focal contacts was verified. HBDC showed numerous well defined stress fibres which give proof of well spread and strongly anchored cells. Porous surfaces encouraged the attachment and spreading of HBDC. Further investigations regarding long term biomaterial/cell interactions in vitro and in vivo are required to confirm the utility of the new biomaterials.

Formation of Ca/P ceramic coatings by Plasma Electrolytic Oxidation (PEO) on Ti6Al4V ELI alloy

NASA Astrophysics Data System (ADS)

Rodriguez-Jaimes, Y.; Naranjo, D. I.; Blanco, S.; García-Vergara, S. J.

2017-12-01

The formation of PEO ceramic coatings on Ti6Al4V ELI alloy was investigated using a phosphate/calcium containing electrolyte at 300 and 400V at 310K for different times. The Plasma Electrolytic Oxidation (PEO) coated specimens were then heat treated at 873 and 1073K for 2 hours. Scanning electron microscopy, Energy Dispersive X-Ray Spectroscopy (EDS) and X-ray diffraction analysis were used to study the composition and the morphology of the ceramic coatings. The corrosion behaviour of the coatings was studied by Electrochemical Impedance Spectroscopy (EIS) in Simulated Body Fluid (SBF). The PEO-treated specimens primarily revealed a porous structure with thickness between 4 and 12μm, according to the voltage and process time used. The coatings are mainly composed of hydroxyapatite; however, as the voltage and anodizing time increase, the Ca/P ratio decreases. Generally, the corrosion resistance of the alloy was improved by the PEO-treated coatings, although the specimens treated at 1073K showed the presence of cracks that reduced the protective effect of the coatings.

In Situ Neutron Diffraction of Rare-Earth Phosphate Proton Conductors Sr/Ca-doped LaPO4 at Elevated Temperatures

NASA Astrophysics Data System (ADS)

Al-Wahish, Amal; Al-Binni, Usama; Bridges, C. A.; Huq, A.; Bi, Z.; Paranthaman, M. P.; Tang, S.; Kaiser, H.; Mandrus, D.

Acceptor-doped lanthanum orthophosphates are potential candidate electrolytes for proton ceramic fuel cells. We combined neutron powder diffraction (NPD) at elevated temperatures up to 800° C , X-ray powder diffraction (XRD) and scanning electron microscopy (SEM) to investigate the crystal structure, defect structure, thermal stability and surface topography. NPD shows an average bond length distortion in the hydrated samples. We employed Quasi-Elastic Neutron Scattering (QENS) and electrochemical impedance spectroscopy (EIS) to study the proton dynamics of the rare-earth phosphate proton conductors 4.2% Sr/Ca-doped LaPO4. We determined the bulk diffusion and the self-diffusion coefficients. Our results show that QENS and EIS are probing fundamentally different proton diffusion processes. Supported by the U.S. Department of Energy.

Light weight phosphate cements

DOEpatents

Wagh, Arun S.; Natarajan, Ramkumar,; Kahn, David

2010-03-09

A sealant having a specific gravity in the range of from about 0.7 to about 1.6 for heavy oil and/or coal bed methane fields is disclosed. The sealant has a binder including an oxide or hydroxide of Al or of Fe and a phosphoric acid solution. The binder may have MgO or an oxide of Fe and/or an acid phosphate. The binder is present from about 20 to about 50% by weight of the sealant with a lightweight additive present in the range of from about 1 to about 10% by weight of said sealant, a filler, and water sufficient to provide chemically bound water present in the range of from about 9 to about 36% by weight of the sealant when set. A porous ceramic is also disclosed.

Influence of calcium on ceramide-1-phosphate monolayers

PubMed Central

Brezesinski, Gerald; Hill, Alexandra; Gericke, Arne

2016-01-01

Summary Ceramide-1-phosphate (C1P) plays an important role in several biological processes, being identified as a key regulator of many protein functions. For instance, it acts as a mediator of inflammatory responses. The mediation of the inflammation process happens due to the interaction of C1P with the C2 domain of cPLA2α, an effector protein that needs the presence of submicromolar concentrations of calcium ions. The aim of this study was to determine the phase behaviour and structural properties of C1P in the presence and absence of millimolar quantities of calcium in a well-defined pH environment. For that purpose, we used monomolecular films of C1P at the soft air/liquid interface with calcium ions in the subphase. The pH was varied to change the protonation degree of the C1P head group. We used surface pressure versus molecular area isotherms coupled with other monolayer techniques as Brewster angle microscopy (BAM), infrared reflection–absorption spectroscopy (IRRAS) and grazing incidence X-ray diffraction (GIXD). The isotherms indicate that C1P monolayers are in a condensed state in the presence of calcium ions, regardless of the pH. At higher pH without calcium ions, the monolayer is in a liquid-expanded state due to repulsion between the negatively charged phosphate groups of the C1P molecules. When divalent calcium ions are added, they are able to bridge the highly charged phosphate groups, enhancing the regular arrangement of the head groups. Similar solidification of the monolayer structure can be seen in the presence of a 150 times larger concentration of monovalent sodium ions. Therefore, calcium ions have clearly a strong affinity for the phosphomonoester of C1P. PMID:26977381

Interpenetrating phase ceramic/polymer composite coatings: Fabrication and characterization

NASA Astrophysics Data System (ADS)

Craig, Bradley Dene

The goals of this thesis research were to fabricate interpenetrating phase composite (IPC) ceramic/polymer coatings and to investigate the effect of the interconnected microstructure on the physical and wear properties of the coatings. IPC coatings with an interpenetrating phase microstructure were successfully fabricated by first forming a porous ceramic with an interconnected microstructure using a chemical bonding route (mainly reacting alpha-alumina (0.3 mum) with orthophosphoric acid to form a phosphate bond). Porosity within these ceramic coatings was easily controlled between 20 and 50 vol. % by phosphoric acid addition, and was measured by a new porosity measurement technique (thermogravimetric volatilization of liquids, or TVL) which was developed. The resulting ceramic preforms were infiltrated with a UV and thermally curable cycloaliphatic epoxide resin and cured. This fabrication route resulted in composite coatings with thicknesses ranging from ˜1mum to 100 mum with complete filling of open pore space. The physical properties of the composite coatings, including microhardness, flexural modulus and wear resistance, were evaluated as a function of processing variables, including orthophosphoric acid content and ceramic phase firing temperature, which affected the microstructure and interparticulate bonding between particles in the coatings. For example, microhardness increased from ˜30 on the Vicker's scale to well over 200 as interparticulate bonding was increased in the ceramic phase. Additionally, Taber wear resistance in the best TPC coatings was found to approach that of fully-densified alumina under certain conditions. Several factors were found to influence the wear mechanism in the IPC coating materials. Forming strong connections between ceramic particles led to up to an order of magnitude increase in the wear resistance. Additionally, coating microhardness and ceramic/polymer interfacial strength were studied and found to be important in determining the wear mechanism and wear resistance of IPC composite coatings. A qualitative theory for wear mechanisms in these coatings was developed. Finally, a series of transparent coatings were developed via a similar processing route, using smaller (˜90 nm) boehmite particles instead of 0.3 mum alpha-alumina. Physical property control was found to mimic that found in opaque coatings, and showed increasing surface adsorption characteristics with increasing phosphoric acid content.

TRIS buffer in simulated body fluid distorts the assessment of glass-ceramic scaffold bioactivity.

PubMed

Rohanová, Dana; Boccaccini, Aldo Roberto; Yunos, Darmawati Mohamad; Horkavcová, Diana; Březovská, Iva; Helebrant, Aleš

2011-06-01

The paper deals with the characterisation of the bioactive phenomena of glass-ceramic scaffold derived from Bioglass® (containing 77 wt.% of crystalline phases Na(2)O·2CaO·3SiO(2) and CaO·SiO(2) and 23 wt.% of residual glass phase) using simulated body fluid (SBF) buffered with tris-(hydroxymethyl) aminomethane (TRIS). A significant effect of the TRIS buffer on glass-ceramic scaffold dissolution in SBF was detected. To better understand the influence of the buffer, the glass-ceramic scaffold was exposed to a series of in vitro tests using different media as follows: (i) a fresh liquid flow of SBF containing tris (hydroxymethyl) aminomethane; (ii) SBF solution without TRIS buffer; (iii) TRIS buffer alone; and (iv) demineralised water. The in vitro tests were provided under static and dynamic arrangements. SBF buffered with TRIS dissolved both the crystalline and residual glass phases of the scaffold and a crystalline form of hydroxyapatite (HAp) developed on the scaffold surface. In contrast, when TRIS buffer was not present in the solutions only the residual glassy phase dissolved and an amorphous calcium phosphate (Ca-P) phase formed on the scaffold surface. It was confirmed that the TRIS buffer primarily dissolved the crystalline phase of the glass-ceramic, doubled the dissolving rate of the scaffold and moreover supported the formation of crystalline HAp. This significant effect of the buffer TRIS on bioactive glass-ceramic scaffold degradation in SBF has not been demonstrated previously and should be considered when analysing the results of SBF immersion bioactivity tests of such systems. Copyright © 2011 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Bonding effectiveness to different chemically pre-treated dental zirconia.

PubMed

Inokoshi, Masanao; Poitevin, André; De Munck, Jan; Minakuchi, Shunsuke; Van Meerbeek, Bart

2014-09-01

The objective of this study was to evaluate the effect of different chemical pre-treatments on the bond durability to dental zirconia. Fully sintered IPS e.max ZirCAD (Ivoclar Vivadent) blocks were subjected to tribochemical silica sandblasting (CoJet, 3M ESPE). The zirconia samples were additionally pre-treated using one of four zirconia primers/adhesives (Clearfil Ceramic Primer, Kuraray Noritake; Monobond Plus, Ivoclar Vivadent; Scotchbond Universal, 3M ESPE; Z-PRIME Plus, Bisco). Finally, two identically pre-treated zirconia blocks were bonded together using composite cement (RelyX Ultimate, 3M ESPE). The specimens were trimmed at the interface to a cylindrical hourglass and stored in distilled water (7 days, 37 °C), after which they were randomly tested as is or subjected to mechanical ageing involving cyclic tensile stress (10 N, 10 Hz, 10,000 cycles). Subsequently, the micro-tensile bond strength was determined, and SEM fractographic analysis performed. Weibull analysis revealed the highest Weibull scale and shape parameters for the 'Clearfil Ceramic Primer/mechanical ageing' combination. Chemical pre-treatment of CoJet (3M ESPE) sandblasted zirconia using Clearfil Ceramic Primer (Kuraray Noritake) and Monobond Plus (Ivoclar Vivadent) revealed a significantly higher bond strength than when Scotchbond Universal (3M ESPE) and Z-PRIME Plus (Bisco) were used. After ageing, Clearfil Ceramic Primer (Kuraray Noritake) revealed the most stable bond durability. Combined mechanical/chemical pre-treatment, the latter with either Clearfil Ceramic Primer (Kuraray Noritake) or Monobond Plus (Ivoclar Vivadent), resulted in the most durable bond to zirconia. As a standard procedure to durably bond zirconia to tooth tissue, the application of a combined 10-methacryloyloxydecyl dihydrogen phosphate/silane ceramic primer to zirconia is clinically highly recommended.

Does 8-methacryloxyoctyl trimethoxy silane (8-MOTS) improve initial bond strength on lithium disilicate glass ceramic?

PubMed

Maruo, Yukinori; Nishigawa, Goro; Yoshihara, Kumiko; Minagi, Shogo; Matsumoto, Takuya; Irie, Masao

2017-03-01

Dental ceramic surfaces are modified with silane coupling agents, such as γ-methacryloxypropyl trimethoxy silane (γ-MPTS), to improve bond strength. For bonding between lithium disilicate glass ceramic and resin cement, the objective was to investigate if 8-methacryloxyoctyl trimethoxy silane (8-MOTS) could yield a similar performance as the widely used γ-MPTS. One hundred and ten lithium disilicate glass ceramic specimens were randomly divided into 11 groups (n=10) according to pretreatment regime. All specimens were pretreated with a different solution composed of one or a combination of these agents: 10 or 20wt% silane coupling agent of γ-MPTS or 8-MOTS, followed by a hydrolysis solution of acetic acid or 10-methacryloyloxydecyl dihydrogen phosphate (10-MDP). Each pretreated surface was luted to a stainless steel rod of 3.6mm diameter and 2.0mm height with resin cement. Shear bond strength between ceramic and cement was measured after 24-h storage in 37°C distilled water. 8-MOTS produced the same bonding performance as γ-MPTS. Both silane coupling agents significantly increased the bond strength of resin cement, depending on their concentration. When activated by 10-MDP hydrolysis solution, 20wt% concentration produced the highest values (γ-MPTS: 24.9±5.1MPa; 8-MOTS: 24.6±7.4MPa). Hydrolysis with acetic acid produced lower bond strengths than with 10-MDP. Silane coupling pretreatment with 8-MOTS increased the initial bond strength between lithium disilicate glass ceramic and resin cement, rendering the same bonding effect as the conventional γ-MPTS. Copyright © 2016 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

αTCP ceramic doped with dicalcium silicate for bone regeneration applications prepared by powder metallurgy method: in vitro and in vivo studies.

PubMed

Velasquez, Pablo; Luklinska, Zofia B; Meseguer-Olmo, Luis; Mate-Sanchez de Val, Jose E; Delgado-Ruiz, Rafael A; Calvo-Guirado, Jose L; Ramirez-Fernandez, Ma P; de Aza, Piedad N

2013-07-01

This study reports on the in vitro and in vivo behavior of α-tricalcium phosphate (αTCP) and also αTCP doped with either 1.5 or 3.0 wt % of dicalcium silicate (C2 S). The ceramics were successfully prepared by powder metallurgy method combined with homogenization and heat treatment procedures. All materials were composed of a single-phase, αTCP in the case of a pure material, or solid solution of C2 S in αTCP for the doped αTCP, which were stable at room temperature. The ceramics were tested for bioactivity in simulated body fluid, cell culture medium containing adult mesenchymal stem cells of human origin, and in animals. Analytical scanning electron microscopy combined with chemical elemental analysis was used and Fourier transform infrared and conventional histology methods. The in vivo behavior of the ceramics matched the in vitro results, independently of the C2 S content in αTCP. Carbonated hydroxyapatite (CHA) layer was formed on the surface and within the inner parts of the specimens in all cases. A fully mineralized new bone growing in direct contact with the implants was found under the in vivo conditions. The bioactivity and biocompatibility of the implants increased with the C2 S content in αTCP. The C2 S doped ceramics also favoured a phase transformation of αTCP into CHA, important for full implant integration during the natural bone healing processes. αTCP ceramic doped with 3.0 wt % C2 S showed the best bioactive in vitro and in vivo properties of all the compositions and hence could be of interest in specific applications for bone restorative purposes. Copyright © 2012 Wiley Periodicals, Inc.

Application of Solidification Theory to Rapid Solidification Processing

DTIC Science & Technology

1984-07-01

solubility; _NiAl -Cr quasibinary alloys ; Rapid solidification ; Solidification theory I’.ASRACT ICfene an roerso aid it 000e..yV SON identify0 by Week...110100a) ~j ~apid solidification allows the production of alloys with new compositions and * uphases and also allows production of improved alloys by...control of microstructure;L and homogeneity. The effect of rapid solidification velocity on the micro- structure of Ag-Cu alloys is comprehensively

Space Station Furnace Facility Core. Requirements definition and conceptual design study. Volume 2: Technical report. Appendix 6: Technical summary reports

NASA Technical Reports Server (NTRS)

1992-01-01

The Space Station Furnace Facility (SSFF) is a modular facility for materials research in the microgravity environment of the Space Station Freedom (SSF). The SSFF is designed for crystal growth and solidification research in the fields of electronic and photonic materials, metals and alloys, and glasses and ceramics and will allow for experimental determination of the role of gravitational forces in the solidification process. The facility will provide a capability for basic scientific research and will evaluate the commercial viability of low-gravity processing of selected technologically important materials. The facility is designed to support a complement of furnace modules as outlined in the Science Capabilities Requirements Document (SCRD). The SSFF is a three rack facility that provides the functions, interfaces, and equipment necessary for the processing of the furnaces and consists of two main parts: the SSFF Core Rack and the two Experiment Racks. The facility is designed to accommodate two experimenter-provided furnace modules housed within the two experiment racks, and is designed to operate these two furnace modules simultaneously. The SCRD specifies a wide range of furnace requirements and serves as the basis for the SSFF conceptual design. SSFF will support automated processing during the man-tended operations and is also designed for crew interface during the permanently manned configuration. The facility is modular in design and facilitates changes as required, so the SSFF is adept to modifications, maintenance, reconfiguration, and technology evolution.

Laser weldability of 21Cr-6Ni-9Mn stainless steel: Part I - Impurity effects and solidifcation mode

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tate, Stephen B.; Javernick, Daniel Anthony; Lienert, Thomas J.

For laser welded type 21Cr-6Ni-9Mn (21-6-9) stainless steels, the relationship between solidification cracking susceptibility and chemical composition was examined, and primary solidification mode (PSM) diagrams were developed to predict solidification mode. Sigmajig testing was used with experimental heats of type 21-6-9 to determine the effect of P and S on solidification cracking w hen primary austenite solidification occurred. Phosphorus showed a larger influence on solidification cracking relative to S, and a relationship of (P+0.2S ) was found for total impurity content. PSM diagrams to predict solidification mode were developed by analyzing welds made at three travel speeds for a widemore » range of 21-6-9 alloys and some other similar alloys. The minimum Cr eq/Ni eq required for primary ferrite solidification increased as travel speed increased, with more alloys showing primary austenite solidification at higher travel rates. Furthermore, as travel speed increased from 21 to 85 mm/s, the average solidification rate increased from 6 to 25 mm/s.« less

Laser weldability of 21Cr-6Ni-9Mn stainless steel: Part I - Impurity effects and solidifcation mode

DOE PAGES

Tate, Stephen B.; Javernick, Daniel Anthony; Lienert, Thomas J.; ...

2016-11-02

For laser welded type 21Cr-6Ni-9Mn (21-6-9) stainless steels, the relationship between solidification cracking susceptibility and chemical composition was examined, and primary solidification mode (PSM) diagrams were developed to predict solidification mode. Sigmajig testing was used with experimental heats of type 21-6-9 to determine the effect of P and S on solidification cracking w hen primary austenite solidification occurred. Phosphorus showed a larger influence on solidification cracking relative to S, and a relationship of (P+0.2S ) was found for total impurity content. PSM diagrams to predict solidification mode were developed by analyzing welds made at three travel speeds for a widemore » range of 21-6-9 alloys and some other similar alloys. The minimum Cr eq/Ni eq required for primary ferrite solidification increased as travel speed increased, with more alloys showing primary austenite solidification at higher travel rates. Furthermore, as travel speed increased from 21 to 85 mm/s, the average solidification rate increased from 6 to 25 mm/s.« less

Biomaterials for periodontal regeneration

PubMed Central

Shue, Li; Yufeng, Zhang; Mony, Ullas

2012-01-01

Periodontal disease is characterized by the destruction of periodontal tissues. Various methods of regenerative periodontal therapy, including the use of barrier membranes, bone replacement grafts, growth factors and the combination of these procedures have been investigated. The development of biomaterials for tissue engineering has considerably improved the available treatment options above. They fall into two broad classes: ceramics and polymers. The available ceramic-based materials include calcium phosphate (eg, tricalcium phosphate and hydroxyapatite), calcium sulfate and bioactive glass. The bioactive glass bonds to the bone with the formation of a layer of carbonated hydroxyapatite in situ. The natural polymers include modified polysaccharides (eg, chitosan,) and polypeptides (collagen and gelatin). Synthetic polymers [eg, poly(glycolic acid), poly(L-lactic acid)] provide a platform for exhibiting the biomechanical properties of scaffolds in tissue engineering. The materials usually work as osteogenic, osteoconductive and osteoinductive scaffolds. Polymers are more widely used as a barrier material in guided tissue regeneration (GTR). They are shown to exclude epithelial downgrowth and allow periodontal ligament and alveolar bone cells to repopulate the defect. An attempt to overcome the problems related to a collapse of the barrier membrane in GTR or epithelial downgrowth is the use of a combination of barrier membranes and grafting materials. This article reviews various biomaterials including scaffolds and membranes used for periodontal treatment and their impacts on the experimental or clinical management of periodontal defect. PMID:23507891

Nano-biphasic calcium phosphate/polyvinyl alcohol composites with enhanced bioactivity for bone repair via low-temperature three-dimensional printing and loading with platelet-rich fibrin

PubMed Central

Wang, Chunmei; Zhang, Shuaishuai; Li, Donglin; Wang, Jimeng; Cao, Tianqing; Bi, Long; Pei, Guoxian

2018-01-01

Background and aim As a newly emerging three-dimensional (3D) printing technology, low-temperature robocasting can be used to fabricate geometrically complex ceramic scaffolds at low temperatures. Here, we aimed to fabricate 3D printed ceramic scaffolds composed of nano-biphasic calcium phosphate (BCP), polyvinyl alcohol (PVA), and platelet-rich fibrin (PRF) at a low temperature without the addition of toxic chemicals. Methods Corresponding nonprinted scaffolds were prepared using a freeze-drying method. Compared with the nonprinted scaffolds, the printed scaffolds had specific shapes and well-connected internal structures. Results The incorporation of PRF enabled both the sustained release of bioactive factors from the scaffolds and improved biocompatibility and biological activity toward bone marrow-derived mesenchymal stem cells (BMSCs) in vitro. Additionally, the printed BCP/PVA/PRF scaffolds promoted significantly better BMSC adhesion, proliferation, and osteogenic differentiation in vitro than the printed BCP/PVA scaffolds. In vivo, the printed BCP/PVA/PRF scaffolds induced a greater extent of appropriate bone formation than the printed BCP/PVA scaffolds and nonprinted scaffolds in a critical-size segmental bone defect model in rabbits. Conclusion These experiments indicate that low-temperature robocasting could potentially be used to fabricate 3D printed BCP/PVA/PRF scaffolds with desired shapes and internal structures and incorporated bioactive factors to enhance the repair of segmental bone defects. PMID:29416332

Nano-biphasic calcium phosphate/polyvinyl alcohol composites with enhanced bioactivity for bone repair via low-temperature three-dimensional printing and loading with platelet-rich fibrin.

PubMed

Song, Yue; Lin, Kaifeng; He, Shu; Wang, Chunmei; Zhang, Shuaishuai; Li, Donglin; Wang, Jimeng; Cao, Tianqing; Bi, Long; Pei, Guoxian

2018-01-01

As a newly emerging three-dimensional (3D) printing technology, low-temperature robocasting can be used to fabricate geometrically complex ceramic scaffolds at low temperatures. Here, we aimed to fabricate 3D printed ceramic scaffolds composed of nano-biphasic calcium phosphate (BCP), polyvinyl alcohol (PVA), and platelet-rich fibrin (PRF) at a low temperature without the addition of toxic chemicals. Corresponding nonprinted scaffolds were prepared using a freeze-drying method. Compared with the nonprinted scaffolds, the printed scaffolds had specific shapes and well-connected internal structures. The incorporation of PRF enabled both the sustained release of bioactive factors from the scaffolds and improved biocompatibility and biological activity toward bone marrow-derived mesenchymal stem cells (BMSCs) in vitro. Additionally, the printed BCP/PVA/PRF scaffolds promoted significantly better BMSC adhesion, proliferation, and osteogenic differentiation in vitro than the printed BCP/PVA scaffolds. In vivo, the printed BCP/PVA/PRF scaffolds induced a greater extent of appropriate bone formation than the printed BCP/PVA scaffolds and nonprinted scaffolds in a critical-size segmental bone defect model in rabbits. These experiments indicate that low-temperature robocasting could potentially be used to fabricate 3D printed BCP/PVA/PRF scaffolds with desired shapes and internal structures and incorporated bioactive factors to enhance the repair of segmental bone defects.

Effects of Iron on Physical and Mechanical Properties, and Osteoblast Cell Interaction in β-Tricalcium Phosphate

PubMed Central

Vahabzadeh, Sahar; Bose, Susmita

2017-01-01

Iron (Fe) is a vital element and its deficiency causes abnormal bone metabolism. We investigated the effects of Fe and its concentration in β-tricalcium phosphate (β-TCP) on physicomechanical properties and in vitro proliferation and differentiation of osteoblasts. Our results showed that Fe addition at concentrations of 0.5 wt. % (0.5 Fe-TCP) and 1.0 wt. % (1.0 Fe-TCP) inhibits the β-TCP to α-TCP phase transformation at sintering temperature of 1250 °C. Addition of 0.25 wt. % Fe (0.25 Fe-TCP) increased the compressive strength of β-TCP from 167.27±16.2 MPa to 227.10±19.3 MPa. After 3 days of culture, surfaces of 0.5 Fe-TCP and 1.0 Fe-TCP samples were covered by osteoblast cells, compared to that of pure and 0.25 Fe-TCP. Cells grew to confluency on all Fe-doped samples after 7 days of culture and monolayer sheetlike cellular structure was found at 11 days. Optical cell density and alkaline phosphatase activity were significantly higher on Fe-doped samples and the highest values were found in 0.5 Fe-TCP samples. Our results show that Fe concentration had significant effect on physical and mechanical properties of TCP ceramics, and also on the in vitro osteoblast cellular interactions in TCP ceramics. PMID:27896489

Ageing of a phosphate ceramic used to immobilize chloride-contaminated actinide waste

DOE Office of Scientific and Technical Information (OSTI.GOV)

Metcalfe, Brian; Donald, Ian W.; Fong, Shirley K.

2009-03-31

At AWE, we have developed a process for the immobilization of ILW waste containing a significant quantity of chloride with Ca 3(PO 4) 2 as the host material. Waste ions are incorporated into two phosphate-based phases, chlorapatite [Ca 5(PO 4) 3Cl] and spodiosite [Ca 2(PO 4)Cl]. Non-active trials performed at AWE with Sm as the actinide surrogate demonstrated the durability of these phases in aqueous solution. Trials of the process, in which actinide-doped materials were used, wer performed at PNNL where the waste form was found to be resistant to aqueous leaching. Initial leach trials conducted on 239Pu / 241Ammore » loaded ceramic at 40°C/28 days gave normalized mass losses of 1.2 x 10 -5 g.m -2 and 2.7 x 10 -3 g.m -2 for Pu and Cl respectively. In order to assess the response of the phases to radiation-induced damage, accelerated ageing trials were performed on samples in which the 239Pu was replaced with 238Pu. No changes to the crystalline structure of the waste were detected in the XRD patterns after the samples had experienced an α radiation dose of 4 x 10 18 g -1. Leach trials showed that there was an increase in the P and Ca release rates but no change in the Pu release rate.« less

Ageing of a phosphate ceramic used to immobilize chloride contaminated actinide waste

DOE Office of Scientific and Technical Information (OSTI.GOV)

Metcalfe, Brian L.; Donald, Ian W.; Fong, Shirley K.

2009-03-31

AWE has developed a process for the immobilization of ILW waste containing a significant quantity of chloride using Ca3(PO4)2 as the host material. Waste ions are incorporated into two phosphate based phases, chlorapatite, Ca5(PO4)3Cl, and spodiosite, Ca2(PO4)Cl. Non-active trials performed at AWE using samarium as the actinide surrogate demonstrated the durability of these phases in aqueous solution. Trials of the process using actinide-doped material were performed at PNNL which confirmed the immobilized wasteform resistant to aqueous leaching. Initial leach trials conducted on 239Pu /241Am loaded ceramic at 40°C/28 days gave normalized mass losses of 1.2 x 10-5 g.m-2 and 2.7more » x 10-3 g.m-2 for Pu and Cl respectively. In order to assess the response of the phases to radiation-induced damage, accelerated ageing trials were performed on samples in which the 239Pu was replaced by 238Pu. No changes to the crystalline structure of the waste were detected using XRD after the samples had experienced a radiation dose of 4 x 1018 α.g-1. Leach trials showed that there had been an increase in the P and Ca release rates but no change in the Pu release rate.« less

Study of structural, electrical, and dielectric properties of phosphate-borate glasses and glass-ceramics

NASA Astrophysics Data System (ADS)

Melo, B. M. G.; Graça, M. P. F.; Prezas, P. R.; Valente, M. A.; Almeida, A. F.; Freire, F. N. A.; Bih, L.

2016-08-01

In this work, phosphate-borate based glasses with molar composition 20.7P2O5-17.2Nb2O5-13.8WO3-34.5A2O-13.8B2O3, where A = Li, Na, and K, were prepared by the melt quenching technique. The as-prepared glasses were heat-treated in air at 800 °C for 4 h, which led to the formation of glass-ceramics. These high chemical and thermal stability glasses are good candidates for several applications such as fast ionic conductors, semiconductors, photonic materials, electrolytes, hermetic seals, rare-earth ion host solid lasers, and biomedical materials. The present work endorses the analysis of the electrical conductivity of the as-grown samples, and also the electrical, dielectric, and structural changes established by the heat-treatment process. The structure of the samples was analyzed using X-Ray powder Diffraction (XRD), Raman spectroscopy, and density measurements. Both XRD and Raman analysis confirmed crystals formation through the heat-treatment process. The electrical ac and dc conductivities, σac and σdc, respectively, and impedance spectroscopy measurements as function of the temperature, varying from 200 to 380 K, were investigated for the as-grown and heat-treated samples. The impedance spectroscopy was measured in the frequency range of 100 Hz-1 MHz.

Derivative effect of laser cladding on interface stability of YSZ@Ni coating on GH4169 alloy: An experimental and theoretical study

NASA Astrophysics Data System (ADS)

Zheng, Haizhong; Li, Bingtian; Tan, Yong; Li, Guifa; Shu, Xiaoyong; Peng, Ping

2018-01-01

Yttria-stabilized zirconia YSZ@Ni core-shell nanoparticles were used to prepare a thermal barrier coating (TBC) on a GH4169 alloy by laser cladding. Microstructural analysis showed that the TBC was composed of two parts: a ceramic and a bonding layer. In places where the ZrO2/Al2O3 eutectic structure was present in the ceramic layer, the Ni atoms diffused into the bonding layer, as confirmed by energy-dispersive X-ray spectroscopy (EDS). The derivative effect of laser cladding results in the original YSZ@Ni core-shell nanoparticles being translated into the Al2O3 crystal, activating the YSZ. The mechanism of ceramic/metal interface cohesion was studied in depth via first-principles and molecular dynamics simulation. The results show that the trend in the diffusion coefficients of Ni, Fe, Al, and Ti is DNi > DFe > DTi > DAl in the melting or solidification process of the material. The enthalpy of formation for Al2O3 is less than that of TiO2, resulting in a thermally grown oxide (TGO) Al2O3 phase transformation. With regard to the electronic structure, the trend in Mulliken population is QO-Ni > QZr-O > QO-Al. Although the bonding is slightly weakened between ZrO2/Al2O3 (QZr-O = 0.158 < QO-Ni = 0.220) compared to that in ZrO2/Ni, TGO Al2O3 can improve the oxidation resistance of the metal matrix. Thus, by comparing the connective and diffusive processes, our findings lay the groundwork for detailed and comprehensive studies of the laser cladding process for the production of composite materials.

Physical properties and morphology of electrospun composite fiber mats of polyhydroxyalkanoate containing nanoclay and tricalcium phosphate additives

NASA Astrophysics Data System (ADS)

Tanadchangsaeng, N.; Boonyagul, S.

2018-05-01

Recently, nanofiber research has gained substantial attention from scientists. In this study, the main component of the nanofiber sheet is polyhydroxyalkanoate (PHA) polymer, which is strong, ductile, flexible and adhesive to human skin. Two major additives of nanofiber sheet that we applied are nanoclay and tricalcium phosphate. The additives are generally synthetic substances that can be chemically synthesized and compatible with tissues body. Nanoclay has a low density, strong, durable to compressive strength and humidity. While, tricalcium phosphate is a calcium phosphate ceramic that is biocompatible to human tissue. From the reasons above, we proposed to choose both nanoclay and tricalcium phosphate for adding into PHA nanofibers for film formation. Thus, this study aims to investigate the morphological and mechanical properties of the fiber mat by using PHA added with various amount of nanoclay and tricalcium phosphate at 0.1%, 1% and 10% by weight, and fabricate nanofiber samples by electrospinning technique. The tested results of scanning electron microscope (SEM) morphology show that the fibers have a uniformed pattern. The PHA containing nanoclay of all additive contents exhibited micrometer diameter distributions, while PHA loaded with 1% tricalcium phosphate still had the nano-scale diameter range, and might be the optimum additive load for further nanometer medical applications. A tensile test was performed to determine the effect of nanoclay and tricalcium phosphate contents on the mechanical properties of the electrospun PHA films, and reflect the level of modularity. With nanoclay components being integrated into the polymer matrix, subsequent reduction in fiber crystallinity was occurred after addition of nanoclay with an increase of modulus value. The results confirmed that PHA fiber mat containing 1% nanoclay may have a potential for using as a rigid scaffold which bearing force loading in human organ system. Whereas, it can be indicated that PHA fiber mat containing 1% tricalcium phosphate might be employed as a flexible scaffold for biomedical materials application due to a high elongation at break value.

Phase-field simulation of weld solidification microstructure in an Al Cu alloy

NASA Astrophysics Data System (ADS)

Farzadi, A.; Do-Quang, M.; Serajzadeh, S.; Kokabi, A. H.; Amberg, G.

2008-09-01

Since the mechanical properties and the integrity of the weld metal depend on the solidification behaviour and the resulting microstructural characteristics, understanding weld pool solidification is of importance to engineers and scientists. Thermal and fluid flow conditions affect the weld pool geometry and solidification parameters. During solidification of the weld pool, a columnar grain structure develops in the weld metal. Prediction of the formation of the microstructure during welding may be an important and supporting factor for technology optimization. Nowadays, increasing computing power allows direct simulations of the dendritic and cell morphology of columnar grains in the molten zone for specific temperature conditions. In this study, the solidification microstructures of the weld pool at different locations along the fusion boundary are simulated during gas tungsten arc welding of Al-3wt%Cu alloy using the phase-field model for the directional solidification of dilute binary alloys. A macroscopic heat transfer and fluid flow model was developed to assess the solidification parameters, notably the temperature gradient and solidification growth rate. The effect of the welding speed is investigated. Computer simulations of the solidification conditions and the formation of a cellular morphology during the directional solidification in gas tungsten arc welding are described. Moreover, the simulation results are compared with existing theoretical models and experimental findings.

The solidification velocity of nickel and titanium alloys

NASA Astrophysics Data System (ADS)

Altgilbers, Alex Sho

2002-09-01

The solidification velocity of several Ni-Ti, Ni-Sn, Ni-Si, Ti-Al and Ti-Ni alloys were measured as a function of undercooling. From these results, a model for alloy solidification was developed that can be used to predict the solidification velocity as a function of undercooling more accurately. During this investigation a phenomenon was observed in the solidification velocity that is a direct result of the addition of the various alloying elements to nickel and titanium. The additions of the alloying elements resulted in an additional solidification velocity plateau at intermediate undercoolings. Past work has shown a solidification velocity plateau at high undercoolings can be attributed to residual oxygen. It is shown that a logistic growth model is a more accurate model for predicting the solidification of alloys. Additionally, a numerical model is developed from simple description of the effect of solute on the solidification velocity, which utilizes a Boltzmann logistic function to predict the plateaus that occur at intermediate undercoolings.

Visualization of solidification front phenomena

NASA Technical Reports Server (NTRS)

Workman, Gary L.; Smith, Guy A.

1993-01-01

Directional solidification experiments have been utilized throughout the Materials Processing in Space Program to provide an experimental platform which minimizes variables in solidification experiments. Because of the wide-spread use of this experimental technique in space-based research, it has become apparent that a better understanding of all the phenomena occurring during solidification can be better understood if direct visualization of the solidification interface were possible.

Synthesis and characterization of cerium containing iron phosphate based glass-ceramics

NASA Astrophysics Data System (ADS)

Deng, Yi; Liao, Qilong; Wang, Fu; Zhu, Hanzhen

2018-02-01

The structure and properties of xCeO2-(100-x)(40Fe2O3-60P2O5), where x = 0, 2, 4, 6 and 8 mol%, glass-ceramics prepared by melting and slow cooling method have been investigated by using X-ray diffraction (XRD), scanning electron microscope (SEM), Fourier transform infrared spectroscopy (FTIR), differential thermal analysis (DTA) and the Product Consistency Test (PCT). The results show that the 40Fe2O3-60P2O5 sample is homogeneously amorphous and the sample containing 2 mol% CeO2 has a small amount of FePO4 phase embedded. For the sample containing up to 4 mol% CeO2, monazite CePO4 and a small amount of FePO4 appear. Spectra analysis show that the structure networks of the glass-ceramics mainly consist of orthophosphate, along with pyrophosphate and a small amount of metaphosphate units. Moreover, the leaching rates of Fe and Ce are about 3.5 × 10-5 g m-2 d-1 and 5.0 × 10-5 g m-2 d-1 respectively after immersion in deionized water at 90 °C for 56 days, indicating their good chemical durability. The conclusions imply that the prepared method may be a promising process to immobilize nuclear waste into glass-ceramic matrix.

Early osteoblast responses to orthopedic implants: Synergy of surface roughness and chemistry of bioactive ceramic coating.

PubMed

Aniket; Reid, Robert; Hall, Benika; Marriott, Ian; El-Ghannam, Ahmed

2015-06-01

Pro-osteogenic stimulation of bone cells by bioactive ceramic-coated orthopedic implants is influenced by both surface roughness and material chemistry; however, their concomitant impact on osteoblast behavior is not well understood. The aim of this study is to investigate the effects of nano-scale roughness and chemistry of bioactive silica-calcium phosphate nanocomposite (SCPC50) coated Ti-6Al-4V on modulating early bone cell responses. Cell attachment was higher on SCPC50-coated substrates compared to the uncoated controls; however, cells on the uncoated substrate exhibited greater spreading and superior quality of F-actin filaments than cells on the SCPC50-coated substrates. The poor F-actin filament organization on SCPC50-coated substrates is thought to be due to the enhanced calcium uptake by the ceramic surface. Dissolution analyses showed that an increase in surface roughness was accompanied by increased calcium uptake, and increased phosphorous and silicon release, all of which appear to interfere with F-actin assembly and osteoblast morphology. Moreover, cell attachment onto the SCPC50-coated substrates correlated with the known adsorption of fibronectin, and was independent of surface roughness. High-throughput genome sequencing showed enhanced expression of extracellular matrix and cell differentiation related genes. These results demonstrate a synergistic relationship between bioactive ceramic coating roughness and material chemistry resulting in a phenotype that leads to early osteoblast differentiation. © 2014 Wiley Periodicals, Inc.

A high performance ceramic-polymer separator for lithium batteries

NASA Astrophysics Data System (ADS)

Kumar, Jitendra; Kichambare, Padmakar; Rai, Amarendra K.; Bhattacharya, Rabi; Rodrigues, Stanley; Subramanyam, Guru

2016-01-01

A three-layered (ceramic-polymer-ceramic) hybrid separator was prepared by coating ceramic electrolyte [lithium aluminum germanium phosphate (LAGP)] over both sides of polyethylene (PE) polymer membrane using electron beam physical vapor deposition (EB-PVD) technique. Ionic conductivities of membranes were evaluated after soaking PE and LAGP/PE/LAGP membranes in a 1 Molar (1M) lithium hexafluroarsenate (LiAsF6) electrolyte in ethylene carbonate (EC), dimethyl carbonate (DMC) and ethylmethyl carbonate (EMC) in volume ratio (1:1:1). Scanning electron microscopy (SEM) and X-ray diffraction (XRD) techniques were employed to evaluate morphology and structure of the separators before and after cycling performance tests to better understand structure-property correlation. As compared to regular PE separator, LAGP/PE/LAGP hybrid separator showed: (i) higher liquid electrolyte uptake, (ii) higher ionic conductivity, (iii) lower interfacial resistance with lithium and (iv) lower cell voltage polarization during lithium cycling at high current density of 1.3 mA cm-2 at room temperature. The enhanced performance is attributed to higher liquid uptake, LAGP-assisted faster ion conduction and dendrite prevention. Optimization of density and thickness of LAGP layer on PE or other membranes through manipulation of PVD deposition parameters will enable practical applications of this novel hybrid separator in rechargeable lithium batteries with high energy, high power, longer cycle life, and higher safety level.

Hydrophobic and Metallophobic Surfaces: Highly Stable Non-wetting Inorganic Surfaces Based on Lanthanum Phosphate Nanorods

NASA Astrophysics Data System (ADS)

Sankar, Sasidharan; Nair, Balagopal N.; Suzuki, Takehiro; Anilkumar, Gopinathan M.; Padmanabhan, Moothetty; Hareesh, Unnikrishnan Nair S.; Warrier, Krishna G.

2016-03-01

Metal oxides, in general, are known to exhibit significant wettability towards water molecules because of the high feasibility of synergetic hydrogen-bonding interactions possible at the solid-water interface. Here we show that the nano sized phosphates of rare earth materials (Rare Earth Phosphates, REPs), LaPO4 in particular, exhibit without any chemical modification, unique combination of intrinsic properties including remarkable hydrophobicity that could be retained even after exposure to extreme temperatures and harsh hydrothermal conditions. Transparent nanocoatings of LaPO4 as well as mixture of other REPs on glass surfaces are shown to display notable hydrophobicity with water contact angle (WCA) value of 120° while sintered and polished monoliths manifested WCA greater than 105°. Significantly, these materials in the form of coatings and monoliths also exhibit complete non-wettability and inertness towards molten metals like Ag, Zn, and Al well above their melting points. These properties, coupled with their excellent chemical and thermal stability, ease of processing, machinability and their versatile photo-physical and emission properties, render LaPO4 and other REP ceramics utility in diverse applications.

Nitrogen and Phosphorus Removal from Wastewater Treatment Plant Effluent via Bacterial Sulfate Reduction in an Anoxic Bioreactor Packed with Wood and Iron

PubMed Central

Yamashita, Takahiro; Yamamoto-Ikemoto, Ryoko

2014-01-01

We investigated the removal of nitrogen and phosphate from the effluent of a sewage treatment plant over a long-term operation in bioreactors packed with different combinations of wood and iron, with a trickling filter packed with foam ceramics for nitrification. The average nitrification rate in the trickling filter was 0.17 kg N/m3∙day and remained at 0.11 kg N/m3∙day even when the water temperature was below 15 °C. The denitrification and phosphate removal rates in the bioreactor packed with aspen wood and iron were higher than those in the bioreactor packed with cedar chips and iron. The bioreactor packed with aspen wood and iron continued to remove nitrate and phosphate for >1200 days of operation. The nitrate removal activity of a biofilm attached to the aspen wood from the bioreactor after 784 days of operation was 0.42 g NO3-N/kg dry weight wood∙ day. There was no increase in the amount of dissolved organic matter in the outflow from the bioreactors. PMID:25247426

Design of calcium phosphate ceramics for drug delivery applications in bone diseases: A review of the parameters affecting the loading and release of the therapeutic substance.

PubMed

Parent, Marianne; Baradari, Hiva; Champion, Eric; Damia, Chantal; Viana-Trecant, Marylène

2017-04-28

Effective treatment of critical-size defects is a key challenge in restorative surgery of bone. The strategy covers the implantation of biocompatible, osteoconductive, bioactive and biodegradable devices which (1) well interact with native tissue, mimic multi-dimensional and hierarchical structure of bone and (2) are able to enhance bone repair, treating post implantation pathologies or bone diseases by local delivery of therapeutic agents. Among different options, calcium phosphate biomaterials are found to be attractive choices, due to their excellent biocompatibility, customisable bioactivity and biodegradability. Several approaches have been established to enhance this material ability to be loaded with a therapeutic agent, in order to obtain an in situ controlled release that meets the clinical needs. This article reviews the most important factors influencing on both drug loading and release capacity of porous calcium phosphate bone substitutes. Characteristics of the carrier, drug/carrier interactions, experimental conditions of drug loading and evaluation of drug delivery are considered successively. Copyright © 2017 Elsevier B.V. All rights reserved.

Hydrophobic and Metallophobic Surfaces: Highly Stable Non-wetting Inorganic Surfaces Based on Lanthanum Phosphate Nanorods.

PubMed

Sankar, Sasidharan; Nair, Balagopal N; Suzuki, Takehiro; Anilkumar, Gopinathan M; Padmanabhan, Moothetty; Hareesh, Unnikrishnan Nair S; Warrier, Krishna G

2016-03-09

Metal oxides, in general, are known to exhibit significant wettability towards water molecules because of the high feasibility of synergetic hydrogen-bonding interactions possible at the solid-water interface. Here we show that the nano sized phosphates of rare earth materials (Rare Earth Phosphates, REPs), LaPO4 in particular, exhibit without any chemical modification, unique combination of intrinsic properties including remarkable hydrophobicity that could be retained even after exposure to extreme temperatures and harsh hydrothermal conditions. Transparent nanocoatings of LaPO4 as well as mixture of other REPs on glass surfaces are shown to display notable hydrophobicity with water contact angle (WCA) value of 120° while sintered and polished monoliths manifested WCA greater than 105°. Significantly, these materials in the form of coatings and monoliths also exhibit complete non-wettability and inertness towards molten metals like Ag, Zn, and Al well above their melting points. These properties, coupled with their excellent chemical and thermal stability, ease of processing, machinability and their versatile photo-physical and emission properties, render LaPO4 and other REP ceramics utility in diverse applications.

Development and Characterization of Biphasic Hydroxyapatite/β-TCP Cements.

PubMed

Gallinetti, Sara; Canal, Cristina; Ginebra, Maria-Pau; Ferreira, J

2014-04-01

Biphasic calcium phosphate bioceramics composed of hydroxyapatite (HA) and β-tricalcium phosphate (β-TCP) have relevant properties as synthetic bone grafts, such as tunable resorption, bioactivity, and intrinsic osteoinduction. However, they have some limitations associated to their condition of high-temperature ceramics. In this work self-setting Biphasic Calcium Phosphate Cements (BCPCs) with different HA/β-TCP ratios were obtained from self-setting α-TCP/β-TCP pastes. The strategy used allowed synthesizing BCPCs with modulated composition, compressive strength, and specific surface area. Due to its higher solubility, α-TCP was fully hydrolyzed to a calcium-deficient HA (CDHA), whereas β-TCP remained unreacted and completely embedded in the CDHA matrix. Increasing amounts of the non-reacting β-TCP phase resulted in a linear decrease of the compressive strength, in association to the decreasing amount of precipitated HA crystals, which are responsible for the mechanical consolidation of apatitic cements. Ca 2+ release and degradation in acidic medium was similar in all the BCPCs within the timeframe studied, although differences might be expected in longer term studies once β-TCP, the more soluble phase was exposed to the surrounding media.

Effect of the calcium to phosphorus ratio on the setting properties of calcium phosphate bone cements.

PubMed

Vlad, M D; Gómez, S; Barracó, M; López, J; Fernández, E

2012-09-01

α-Tricalcium phosphate (α-TCP) has become the main reactant of most experimental and commercial ceramic bone cements. It has calcium-to-phosphorus (Ca/P) ratio of 1.50. The present study expands and reports on the microstructures and mechanical properties of calcium phosphate (CP) cements containing sintered monolithic reactants obtained in the interval 1.29 < Ca/P < 1.77. The study focuses on their cement setting and hardening properties as well as on their microstructure and crystal phase evolution. The results showed that: (a) CP-cements made with reactants with Ca/P ratio other than 1.50 have longer setting and lower hardening properties; (b) CP-cements reactivity was clearly affected by the Ca/P ratio of the starting reactant; (c) reactants with Ca/P < 1.50 were composed of several phases, calcium pyrophosphate and α- and β-TCP. Similarly, reactants with Ca/P > 1.50 were composed of α-TCP, tetracalcium phosphate and hydroxyapatite; (d) only the reactant with Ca/P = 1.50 was monophasic and was made of α-TCP, which transformed during the setting into calcium deficient hydroxyapatite; (e) CP-cements developed different crystal microstructures with specific features depending on the Ca/P ratio of the starting reactant.

Partitioning of dopant cations between β-tricalcium phosphate and fluorapatite

NASA Astrophysics Data System (ADS)

Jay, E. E.; Mallinson, P. M.; Fong, S. K.; Metcalfe, B. L.; Grimes, R. W.

2011-07-01

Mixed crystalline phase composite ceramics offer the possibility of partitioning defect species between the phases as well as occupancy of specific sites within a given phase. Here we use atomic scale simulations to study the site preference of an extensive range of divalent and trivalent substitutional ions across the five cation sites in β-tricalcium phosphate ( β-TCP) and the two cations sites in fluorapatite (FAp). This study indicates that in β-TCP small dopant species occupy the smaller of the five cation sites and vice versa. Conversely, in FAp, small divalent species occupy the nominally larger Ca(1) site while larger cations occupy the Ca(2) site. Partition energies between the two phases indicate that divalent species strongly segregate to β-TCP as do Al 3+ and Ga 3+, whereas all other (larger) trivalent ions exhibit little preference.

Microgravity Science and Applications Program tasks, 1987 revision

NASA Technical Reports Server (NTRS)

1988-01-01

A compilation is presented of the active research tasks as of the end of the FY87 of the Microgravity Science and Applications Program, NASA-Office of Space Science and Applications, involving several NASA centers and other organizations. An overview is provided of the program scope for managers and scientists in industry, university, and government communities. An introductory description is provided of the program along with the strategy and overall goal, identification of the organizational structures and people involved, and a description of each task. A list of recent publications is also provided. The tasks are grouped into six major categories: Electronic Materials; Solidification of Metals, Alloys, and Composites; Fluid Dynamics and Transport Phenomena; Biotechnology; Glasses and Ceramics; and Combustion. Other categories include Experimental Technology, General Studies and Surveys; Foreign Government Affiliations; Industrial Affiliations; and Physics and Chemistry Experiments (PACE). The tasks are divided into ground based and flight experiments.

A study of metal-ceramic wettability in SiC-Al using dynamic melt infiltration of SiC

NASA Technical Reports Server (NTRS)

Asthana, R.; Rohatgi, P. K.

1993-01-01

Pressure-assisted infiltration with a 2014 Al alloy of plain and Cu-coated single crystal platelets of alpha silicon carbide was used to study particulate wettability under dynamic conditions relevant to pressure casting of metal-matrix composites. The total penetration length of infiltrant metal in porous compacts was measured at the conclusion of solidification as a function of pressure, infiltration time, and SiC size for both plain and Cu-coated SiC. The experimental data were analyzed to obtain a threshold pressure for the effect of melt intrusion through SiC compacts. The threshold pressure was taken either directly as a measure of wettability or converted to an effective wetting angle using the Young-Laplace capillary equation. Cu coating resulted in partial but beneficial improvements in wettability as a result of its dissolution in the melt, compared to uncoated SiC.

Materials Science Research Rack Onboard the International Space Station

NASA Technical Reports Server (NTRS)

Reagan, Shawn E.; Lehman, John R.; Frazier, Natalie C.

2014-01-01

The Materials Science Research Rack (MSRR) is a highly automated facility developed in a joint venture/partnership between NASA and ESA center dot Allows for the study of a variety of materials including metals, ceramics, semiconductor crystals, and glasses onboard the International Space Station (ISS) center dot Multi-user facility for high temperature materials science research center dot Launched on STS-128 in August 2009, and is currently installed in the U.S. Destiny Laboratory Module ?Research goals center dot Provide means of studying materials processing in space to develop a better understanding of the chemical and physical mechanisms involved center dot Benefit materials science research via the microgravity environment of space where the researcher can better isolate the effects of gravity during solidification on the properties of materials center dot Use the knowledge gained from experiments to make reliable predictions about conditions required on Earth to achieve improved materials

Laser surface alloying on aluminum and its alloys: A review

NASA Astrophysics Data System (ADS)

Chi, Yiming; Gu, Guochao; Yu, Huijun; Chen, Chuanzhong

2018-01-01

Aluminum and its alloys have been widely used in aerospace, automotive and transportation industries owing to their excellent properties such as high specific strength, good ductility and light weight. Surface modification is of crucial importance to the surface properties of aluminum and its alloys since high coefficient of friction, wear characteristics and low hardness have limited their long term performance. Laser surface alloying is one of the most effective methods of producing proper microstructure by means of non-equilibrium solidification which results from rapid heating and cooling. In this paper, the influence of different processing parameters, such as laser power and scanning velocity is discussed. The developments of various material systems including ceramics, metals or alloys, and metal matrix composites (MMCs) are reviewed. The microstructure, hardness, wear properties and other behaviors of laser treated layer are analyzed. Besides, the existing problems during laser surface treatment and the corresponding solutions are elucidated and the future developments are predicted.

Silicon-on-ceramic Process: Silicon Sheet Growth and Device Development for the Large-area Silicon Sheet and Cell Development Tasks of the Low-cost Solar Array Project

NASA Technical Reports Server (NTRS)

Chapman, P. W.; Zook, J. D.; Heaps, J. D.; Grung, B. L.; Koepke, B.; Schuldt, S. B.

1979-01-01

Significant progress is reported in fabricating a 4 sq cm cell having a 10.1 percent conversion efficiency and a 10 sq cm cell having a 9.2 percent conversion efficiency. The continuous (SCIM) coater succeeded in producing a 16 sq cm coating exhibiting unidirectional solidification and large grain size. A layer was grown at 0.2 cm/sec in the experimental coater which was partially dendritic but also contained a large smooth area approximately 100 micron m thick. The dark characteristic measurements of a typical SCC solar cell yield shunt resistance values of 10K ohms and series resistance values and 0.4 ohm. The production dip-coater is operating at over 50 percent yield in terms of good cell quality material. The most recent run yielded 13 good substrates out of 15.

Microgravity Science and Applications Program tasks, 1988 revision

NASA Technical Reports Server (NTRS)

1989-01-01

The active research tasks as of the end of the fiscal year 1988 of the Microgravity Science and Applications Program, NASA-Office of Space Science and Applications, involving several NASA centers and other organizations are compiled. The purpose is to provide an overview of the program scope for managers and scientists in industry, university, and government communities. Also included are an introductory description of the program, the strategy and overall goal, identification of the organizational structures and people involved, and a description of each task. A list of recent publications is provided. The tasks are grouped into six major categories: electronic materials; solidification of metals, alloys, and composites; fluid dynamics and transport phenomena; biotechnology; glasses and ceramics; and combustion. Other categories include experimental technology, general studies and surveys; foreign government affiliations; industrial affiliations; and Physics And Chemistry Experiments (PACE). The tasks are divided into ground-based and flight experiments.

Study of ceramic products and processing techniques in space. [using computerized simulation

NASA Technical Reports Server (NTRS)

Markworth, A. J.; Oldfield, W.

1974-01-01

An analysis of the solidification kinetics of beta alumina in a zero-gravity environment was carried out, using computer-simulation techniques, in order to assess the feasibility of producing high-quality single crystals of this material in space. The two coupled transport processes included were movement of the solid-liquid interface and diffusion of sodium atoms in the melt. Results of the simulation indicate that appreciable crystal-growth rates can be attained in space. Considerations were also made of the advantages offered by high-quality single crystals of beta alumina for use as a solid electrolyte; these clearly indicate that space-grown materials are superior in many respects to analogous terrestrially-grown crystals. Likewise, economic considerations, based on the rapidly expanding technological applications for beta alumina and related fast ionic conductors, reveal that the many superior qualities of space-grown material justify the added expense and experimental detail associated with space processing.

Chitosan-glycerol phosphate/blood implants improve hyaline cartilage repair in ovine microfracture defects.

PubMed

Hoemann, Caroline D; Hurtig, Mark; Rossomacha, Evgeny; Sun, Jun; Chevrier, Anik; Shive, Matthew S; Buschmann, Michael D

2005-12-01

Microfracture is a surgical procedure that is used to treat focal articular cartilage defects. Although joint function improves following microfracture, the procedure elicits incomplete repair. As blood clot formation in the microfracture defect is an essential initiating event in microfracture therapy, we hypothesized that the repair would be improved if the microfracture defect were filled with a blood clot that was stabilized by the incorporation of a thrombogenic and adhesive polymer, specifically, chitosan. The objectives of the present study were to evaluate (1) blood clot adhesion in fresh microfracture defects and (2) the quality of the repair, at six months postoperatively, of microfracture defects that had been treated with or without chitosan-glycerol phosphate/blood clot implants, using a sheep model. In eighteen sheep, two 1-cm2 full-thickness chondral defects were created in the distal part of the femur and treated with microfracture; one defect was made in the medial femoral condyle, and the other defect was made in the trochlea. In four sheep, microfracture defects were created bilaterally; the microfracture defects in one knee received no further treatment, and the microfracture defects in the contralateral knee were filled with chitosan-glycerol phosphate/autologous whole blood and the implants were allowed to solidify. Fresh defects in these four sheep were collected at one hour postoperatively to compare the retention of the chitosan-glycerol phosphate/blood clot with that of the normal clot and to define the histologic characteristics of these fresh defects. In the other fourteen sheep, microfracture defects were made in only one knee and either were left untreated (control group; six sheep) or were treated with chitosan-glycerol phosphate/blood implant (treatment group; eight sheep), and the quality of repair was assessed histologically, histomorphometrically, and biochemically at six months postoperatively. In the defects that were examined one hour postoperatively, chitosan-glycerol phosphate/blood clots showed increased adhesion to the walls of the defects as compared with the blood clots in the untreated microfracture defects. After histological processing, all blood clots in the control microfracture defects had been lost, whereas chitosanglycerol phosphate/blood clot adhered to and was partly retained on the surfaces of the defect. At six months, defects that had been treated with chitosan-glycerol phosphate/blood were filled with significantly more hyaline repair tissue (p < 0.05) compared with control defects. Repair tissue from medial femoral condyle defects that had been treated with chitosan-glycerol phosphate/blood contained more cells and more collagen compared with control defects and showed complete restoration of glycosaminoglycan levels. Solidification of a chitosan-glycerol phosphate/blood implant in microfracture defects improved cartilage repair compared with microfracture alone by increasing the amount of tissue and improving its biochemical composition and cellular organization.

Wear resistance and compression strength of ceramics tested in fluoride environments.

PubMed

Theodoro, Guilherme Teixeira; Fiorin, Lívia; Moris, Izabela Cristina Maurício; Rodrigues, Renata Cristina Silveira; Ribeiro, Ricardo Faria; Faria, Adriana Cláudia Lapria

2017-01-01

Dental ceramics have been widely used because of aesthetic, but wear is still questioned. There are relates that ceramic surface is prone to degradation by acidulated fluoride, that can increase wear rates. The aim of this study was to evaluate the effect of neutral and acidulated fluoride gel, used as preventive agents for professional use, at wear and compression strength of dental ceramics IPS e.max ZirPress (ZIR), IPS Empress Esthetic (EMP) e IPS Inline POM (POM). For this, 30 crowns and 30 disks were obtained by heat-pressing. Crowns and disks were submitted to two-body wear test at machine of mechanical loading, simulating occlusion, lateral movement and disocclusion. It was performed 300,000 cycles at 1Hz frequency under 20N load, to simulate 1 year of mastication. Samples were totally immersed during the test and were divided into three groups according to the gel used for immersion (n=10): control, neutral (sodium fluoride 2%) and acidulated (acidulated phosphate fluoride 1.23%). Samples (crowns and disks) were analyzed for vertical height loss after the test using, respectively, profile projector and stereomicroscope. Roughness of worn surface of crowns and disks was evaluated by laser confocal microscopy. Data of height loss and roughness were evaluated by two-way ANOVA and Bonferroni's test. A crown/disk of each group was analyzed by scanning electronic microscopy. After wear resistance tests, crowns were cemented to their abutments and submitted to compressive load at 30° angulation and 1mm/min speed. Type of failures was compared by qui-square test. Ceramic EMP worn less while ZIR worn more. Control gel worn more at crowns while acidulated gel worn more at disks. Surface roughness of samples tested at acidulated gel was significantly lower. Type of failures found at compression resistance tests was affected by ceramic type, but not by gel used. The results suggest that ceramic and fluoride gel affect wear and roughness of worn surface while type of failure is only affected by ceramic. Copyright © 2016 Elsevier Ltd. All rights reserved.

Simple Signaling Molecules for Inductive Bone Regenerative Engineering

PubMed Central

Nelson, Stephen J.; Deng, Meng; Sethuraman, Swaminathan; Doty, Stephen B.; Lo, Kevin W. H.; Khan, Yusuf M.; Laurencin, Cato T.

2014-01-01

With greater than 500,000 orthopaedic procedures performed in the United States each year requiring a bone graft, the development of novel graft materials is necessary. We report that some porous polymer/ceramic composite scaffolds possess intrinsic osteoinductivity as shown through their capacity to induce in vivo host osteoid mineralization and in vitro stem cell osteogenesis making them attractive synthetic bone graft substitutes. It was discovered that certain low crystallinity ceramics partially dissociate into simple signaling molecules (i.e., calcium and phosphate ions) that induce stem cells to endogenously produce their own osteoinductive proteins. Review of the literature has uncovered a variety of simple signaling molecules (i.e., gases, ions, and redox reagents) capable of inducing other desirable stem cell differentiation through endogenous growth factor production. Inductive simple signaling molecules, which we have termed inducerons, represent a paradigm shift in the field of regenerative engineering where they can be utilized in place of recombinant protein growth factors. PMID:25019622

Atomistic modeling and experimental studies of radiation damage in monazite-type LaPO4 ceramics

NASA Astrophysics Data System (ADS)

Ji, Yaqi; Kowalski, Piotr M.; Neumeier, Stefan; Deissmann, Guido; Kulriya, Pawan K.; Gale, Julian D.

2017-02-01

We simulated the threshold displacement energies (Ed), the related displacement and defect formation probabilities, and the energy barriers in LaPO4 monazite-type ceramics. The obtained Ed values for La, P, O primary knock-on atoms (PKA) are 56 eV, 75 eV and 8 eV, respectively. We found that these energies can be correlated with the energy barriers that separate the defect from the initial states. The Ed values are about twice the values of energy barriers, which is explained through an efficient dissipation of the PKA kinetic energy in the considered system. The computed Ed were used in simulations of the extent of radiation damage in La0.2Gd0.8PO4 solid solution, investigated experimentally. We found that this lanthanide phosphate fully amorphises in the ion beam experiments for fluences higher than ∼1013 ions/cm2.

Microstructure Evolution in the Presence of Constraints and Implications on the Properties of Mg - Li and Nb - Al Composites

DTIC Science & Technology

1991-05-30

alloys and composites Solidification experiments with Succinonitrile-acetone system Experimerts with Salol I Directional Solidification of Mg-Li alloys ...Directional Solidification of Mg-Li Composites Microstructural Analysis and Modeling Combustion Synthesis Principles ( theory ) Nb-AI alloys made by...Combustion Synthesis Nb-AI - NbB composites made by Combustion Synthesis Directional Solidification of Nb-AI Alloys Directional Solidification of Nb- Al

The influence of gravity level during directional solidification of immiscible alloys

NASA Technical Reports Server (NTRS)

Andrews, J. B.; Schmale, A. L.; Sandlin, A. C.

1992-01-01

During directional solidification of immiscible (hypermonotectic) alloys it is theoretically possible to establish a stable macroscopically-planar solidification front, and thus avoid sedimentation. Unfortunately, convective instabilities often occur which interfere with the directional solidification process. In this paper, stability conditions are discussed and results presented from directional solidification studies carried out aboard NASA's KC-135 zero-g aircraft. Samples were directionally solidified while the effective gravity level was varied from approximately 0.01 g for 25 s to 1.8 g for 45 s. Dramatic variations in microstructure were observed with gravity level during solidification.

Tranpsort phenomena in solidification processing of functionally graded materials

NASA Astrophysics Data System (ADS)

Gao, Juwen

A combined numerical and experimental study of the transport phenomena during solidification processing of metal matrix composite functionally graded materials (FGMs) is conducted in this work. A multiphase transport model for the solidification of metal-matrix composite FGMs has been developed that accounts for macroscopic particle segregation due to liquid-particle flow and particle-solid interactions. An experimental study has also been conducted to gain physical insight as well as to validate the model. A novel method to in-situ measure the particle volume fraction using fiber optic probes is developed for transparent analogue solidification systems. The model is first applied to one-dimensional pure matrix FGM solidification under gravity or centrifugal field and is extensively validated against the experimental results. The mechanisms for the formation of particle concentration gradient are identified. Two-dimensional solidification of pure matrix FGM with convection is then studied using the model as well as experiments. The interaction among convection flow, solidification process and the particle transport is demonstrated. The results show the importance of convection in the particle concentration gradient formation. Then, simulations for alloy FGM solidification are carried out for unidirectional solidification as well as two-dimensional solidification with convection. The interplay among heat and species transport, convection and particle motion is investigated. Finally, future theoretical and experimental work is outlined.

Modulation of mesenchymal stem cell behavior by nano- and micro-sized β-tricalcium phosphate particles in suspension and composite structures

NASA Astrophysics Data System (ADS)

Smoak, Mollie; Hogan, Katie; Kriegh, Lisa; Chen, Cong; Terrell, LeKeith B.; Qureshi, Ammar T.; Todd Monroe, W.; Gimble, Jeffrey M.; Hayes, Daniel J.

2015-04-01

Interest has grown in the use of microparticles and nanoparticles for modifying the mechanical and biological properties of synthetic bone composite structures. Micro- and nano-sized calcium phosphates are of interest for their osteoinductive behavior. Engineered composites incorporating polymers and ceramics, such as poly-l-lactic acid (PLLA) and beta-tricalcium phosphate (β-TCP), for bone tissue regeneration have been well investigated for their proliferative and osteoinductive abilities. Only limited research has been done to investigate the effects of different sizes of β-TCP particles on human mesenchymal stromal cell behavior. As such, the aim of this study was to investigate the modulations of human adipose-derived stem cell (hASCs) behavior within cell/particle and cell/composite systems as functions of particle size, concentration, and exposure time. The incorporation of nanoscale calcium phosphate resulted in improved mechanical properties and osteogenic behavior within the scaffold compared to the microscale calcium phosphate additives. Particle exposure results indicate that cytotoxicity on hASCs correlates inversely with particle size and increases with the increasing exposure time and particle concentration. Composites with increasing β-TCP content, whether microparticles or nanoparticles, were less toxic than colloidal micro- and nano-sized β-TCP particles directly supplied to hASCs. The difference in viability observed as a result of varying exposure route is likely related to the increased cell-particle interactions in the direct exposure compared to the particles becoming trapped within the scaffold/polymer matrix.

Effect of electrical polarization of hydroxyapatite ceramics on new bone formation.

PubMed

Itoh, S; Nakamura, S; Kobayashi, T; Shinomiya, K; Yamashita, K; Itoh, S

2006-03-01

Large surface charges can be induced on hydroxyapatite (HAp) ceramics by proton transport polarization, but this does not affect beta-tricalcium phosphate (TCP) because of its low polarizability. We wished to examine differences in osteogenic cell activity and new bone growth between positively or negatively surface-charged HAp and HAp/TCP plates using a calvarial bone defect model. In the first group of rats, test pieces were placed with their positively charged surfaces face down on the dura mater. In the second group, test pieces were placed with their negatively charged surfaces face down on the dura mater. A third group received noncharged test pieces. Histological examination, including enzymatic staining for osteoblasts and osteoclasts, was carried out. While no bone formation was observed at the pericranium, direct bone formation on the cranial bone debris and new bone growth expanded from the margins of the sites of injury to bridge across both the positively and negatively charged surfaces of HAp and HAp/TCP plates occurred. Electrical polarization of implanted plates, including positive charge, led to enhanced osteoblast activity, though decreased osteoclast activity was seen on the positively charged plate surface. Thus, polarization of HAp ceramics may modulate new bone formation and resorption.

Bioactive Wollastonite-Diopside Foams from Preceramic Polymers and Reactive Oxide Fillers

PubMed Central

Fiocco, Laura; Elsayed, Hamada; Ferroni, Letizia; Gardin, Chiara; Zavan, Barbara; Bernardo, Enrico

2015-01-01

Wollastonite (CaSiO3) and diopside (CaMgSi2O6) silicate ceramics have been widely investigated as highly bioactive materials, suitable for bone tissue engineering applications. In the present paper, highly porous glass-ceramic foams, with both wollastonite and diopside as crystal phases, were developed from the thermal treatment of silicone polymers filled with CaO and MgO precursors, in the form of micro-sized particles. The foaming was due to water release, at low temperature, in the polymeric matrix before ceramic conversion, mainly operated by hydrated sodium phosphate, used as a secondary filler. This additive proved to be “multifunctional”, since it additionally favored the phase development, by the formation of a liquid phase upon firing, in turn promoting the ionic interdiffusion. The liquid phase was promoted also by the incorporation of powders of a glass crystallizing itself in wollastonite and diopside, with significant improvements in both structural integrity and crushing strength. The biological characterization of polymer-derived wollastonite-diopside foams, to assess the bioactivity of the samples, was performed by means of a cell culture test. The MTT assay and LDH activity tests gave positive results in terms of cell viability.

The effect of luting media on the fracture resistance of a flame sprayed all-ceramic crown.

PubMed

Casson, A M; Glyn Jones, J C; Youngson, C C; Wood, D J

2001-11-01

This in vitro study investigated the effect of selected luting media on the fracture resistance of a flame-sprayed all-ceramic crown. Three groups of 10 human upper premolar teeth were prepared for crowning using a standardised technique. Flame sprayed crowns were fabricated and cemented onto the preparations using zinc phosphate (ZPC), glass polyalkenoate (GPC) or composite luting cement (CLC). During crown seating, a pressure perfusion system simulated pulpal fluid outflow equivalent to 300mm of H2O. Compressive fracture resistance was determined for each group using a Universal Testing Machine with a crosshead speed of 1mm min(-1). A group of unrestored teeth acted as a control. The fracture resistance of the groups ranked as follows: ZPC>CLC>GPC=unrestored teeth. The difference between the fracture resistance of ZPC and CLC groups and the control group was statistically significant. The mode of fracture between the luted crowns and natural crowns was markedly different. When tested in compression, a new, flame-sprayed all-ceramic crown, when luted in place using ZPC, GPC or CLC, could produce strengths comparable to or greater than natural unrestored teeth. The luting agent used significantly affected the recorded fracture loads.

Short-term implantation effects of a DCPD-based calcium phosphate cement.

PubMed

Frayssinet, P; Gineste, L; Conte, P; Fages, J; Rouquet, N

1998-06-01

Calcium phosphate cements can be handled in paste form and set in a wet medium after precipitation of calcium phosphate crystals in the implantation site. Depending on the products entering into the chemical reaction leading to the precipitation of calcium phosphates, different phases can be obtained with different mechanical properties, setting times and injectability. We tested a cement composed of a powder, containing beta-tricalcium phosphate (beta-TCP) and sodium pyrophosphate mixed with a solution of phosphoric and sulphuric acids. The cement set under a dicalcium phosphate dihydrate (DCPD)-based matrix containing beta-TCP particles. This was injected with a syringe into a defect drilled in rabbit condyles, the control being an identical defect left empty in the opposite condyle. The condyles were analysed histologically 2, 6 and 18 weeks after implantation. After injection into the bone defect the cement set and formed a porous calcium phosphate structure. Two different calcium phosphate phases with different solubility rates could be identified by scanning electron microscopy (SEM) observation. The less-soluble fragments could be degraded by cell phagocytosis in cell compartments of low pH or integrated in the newly formed bone matrix. The degradation rate of the material was relatively high but compatible with the ingrowth of bone trabeculae within the resorbing material. The ossification process was different from the creeping substitution occurring at the ceramic contact. Bone did not form directly at the cement surface following the differentiation of osteoblasts at the material surface. The trabeculae came to the material surface from the edges of the implantation site. Bone formation in the implantation site was significantly higher than in the control region during the first week of implantation. In conclusion, this material set in situ was well tolerated, inducing a mild foreign-body reaction, which did not impair its replacement by newly formed bone within a few weeks.

On the Role of Mantle Overturn during Magma Ocean Solidification

NASA Astrophysics Data System (ADS)

Boukaré, C. E.; Parmentier, E.; Parman, S. W.

2017-12-01

Solidification of potential global magma ocean(s) (MO) early in the history of terrestrial planets may play a key role in the evolution of planetary interiors by setting initial conditions for their long-term evolution. Constraining this initial structure of solid mantles is thus crucial but remains poorly understood. MO fractional crystallization has been proposed to generate gravitationally unstable Fe-Mg chemical stratification capable of driving solid-state mantle overturn. Fractional solidification and overturn hypothesis, while only an ideal limiting case, can explain important geochemical features of both the Moon and Mars. Current overturn models consider generally post-MO overturn where the cumulate pile remains immobile until the end of MO solidification. However, if the cumulate pile overturns during MO solidification, the general picture of early planet evolution might differ significantly from the static crystallization models. We show that the timing of mantle overturn can be characterized with a dimensionless number measuring the ratio of the MO solidification time and the purely compositional overturn timescale. Syn-solidification overturn occurs if this dimensionless parameter, Rc, exceeds a critical value. Rc is mostly affected by the competition between the MO solidification time and mantle viscosity. Overturn that occurs during solidification can result in smaller scales of mantle chemical heterogeneity that could persist for long times thus influencing the whole evolution of a planetary body. We will discuss the effects of compaction/percolation on mantle viscosity. If partially molten cumulate do not have time to compact during MO solidification, viscosity of cumulates would be significantly lower as the interstitcial melt fraction would be large. Both solid mantle remelting during syn-solidification overturn and porous convection of melt retained with the cumulates are expected to reduce the degree of fractional crystallization. Syn-solidification overturn of a sluggish mantle can thus be an alternative to solid-state post-MO solidification overturn.

Modelling directional solidification

NASA Technical Reports Server (NTRS)

Wilcox, William R.

1991-01-01

The long range goal of this program is to develop an improved understanding of phenomena of importance to directional solidification and to enable explanation and prediction of differences in behavior between solidification on Earth and in space. Current emphasis is on determining the influence of perturbations on directional solidification.

Improved Crystal Quality By Detached Solidification in Microgravity

NASA Technical Reports Server (NTRS)

Regel, Liya L.; Wilcox, William R.; Wang, Yaz-Hen; Wang, Jian-Bin

2003-01-01

Many microgravity directional solidification experiments yielded ingots with portions that grew without contacting the ampoule wall, leading to greatly improved crystallographic perfection. Our long term goals have been: (1) To develop a complete understanding of all of the phenomena of detached solidification.; (2) To make it possible to achieve detached solidification reproducibly; (3) To increase crystallographic perfection through detached solidification. We have three major achievements to report here: (1) We obtained a new material balance solution for the Moving Meniscus Model of detached solidification. This solution greatly clarifies the physics as well as the roles of the parameters in the system; (2) We achieved detached solidification of InSb growing on earth in BN-coated ampoules; (3) We performed an extensive series of experiments on freezing water that showed how to form multiple gas bubbles or tubes on the ampoule wall. However, these did not propagate around the wall and lead to fully detached solidification unless the ampoule wall was extremely rough and non-wetted.

Relationships Between Solidification Parameters in A319 Aluminum Alloy

NASA Astrophysics Data System (ADS)

Vandersluis, E.; Ravindran, C.

2018-03-01

The design of high-performance materials depends on a comprehensive understanding of the alloy-specific relationships between solidification and properties. However, the inconsistent use of a particular solidification parameter for presenting materials characterization in the literature impedes inter-study comparability and the interpretation of findings. Therefore, there is a need for accurate expressions relating the solidification parameters for each alloy. In this study, A319 aluminum alloy castings were produced in a permanent mold with various preheating temperatures in order to control metal cooling. Analysis of the cooling curve for each casting enabled the identification of its liquidus, Al-Si eutectic, and solidus temperatures and times. These values led to the calculation of the primary solidification rate, total solidification rate, primary solidification time, and local solidification time for each casting, which were related to each other as well as to the average casting SDAS and material hardness. Expressions for each of their correlations have been presented with high coefficients of determination, which will aid in microstructural prediction and casting design.

Surface modification of ceramic and metallic alloy substrates by laser raster-scanning

NASA Astrophysics Data System (ADS)

Ramos Grez, Jorge Andres

This work describes the feasibility of continuous wave laser-raster scan-processing under controlled atmospheric conditions as employed in three distinct surface modification processes: (a) surface roughness reduction of indirect-Selective Laser Sintered 420 martensitic stainless steel-40 wt. % bronze infiltrated surfaces; (b) Si-Cr-Hf-C coating consolidation over 3D carbon-carbon composites cylinders; (c) dendritic solidification structures of Mar-M 247 confined powder precursor grown from polycrystalline Alloy 718 substrates. A heat transfer model was developed to illustrate that the aspect ratio of the laser scanned pattern and the density of scanning lines play a significant role in determining peak surface temperature, heating and cooling rates and melt resident times. Comprehensive characterization of the surface of the processed specimens was performed using scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), optical metallography, X-ray diffraction (XRD), and, in certain cases, tactile profilometry. In Process (a), it was observed that a 24% to 37% roughness Ra reduction could be accomplished from the as-received value of 2.50+/-0.10 microns for laser energy densities ranging from 350 to 500 J/cm2. In Process (b), complete reactive wetting of carbon-carbon composite cylinders surface was achieved by laser melting a Si-Cr-Hf-C slurry. Coatings showed good thermal stability at 1000°C in argon, and, when tested in air, a percent weight reduction rate of -6.5 wt.%/hr was achieved. A soda-glass overcoat applied over the coated specimens by conventional means revealed a percent weight reduction rate between -1.4 to -2.2 wt.%/hr. Finally, in Process (c), microstructure of the Mar-M 247 single layer deposits, 1 mm in height, grown on Alloy 718 polycrystalline sheets, resulted in a sound metallurgical bond, low porosity, and uniform thickness. Polycrystalline dendrites grew preferentially along the [001] direction from the substrate up to 400 microns. Above that height, dendrites appear to shift towards the [100] growth direction driven by the thermal gradient and solidification front velocity. This research demonstrated that surface modification by high speed raster-scanning a high power laser beam under controlled atmospheric conditions is a feasible and versatile technique that can accomplish diverse purposes involving metallic as well as ceramic surfaces.

Modeling of Detached Solidification

NASA Technical Reports Server (NTRS)

Regel, Liya L.; Wilcox, William R.; Popov, Dmitri

1997-01-01

Our long term goal is to develop techniques to achieve detached solidification reliably and reproducibly, in order to produce crystals with fewer defects. To achieve this goal it is necessary to understand thoroughly the physics of detached solidification. It was the primary objective of the current project to make progress toward this complete understanding. 'Me products of this grant are attached. These include 4 papers and a preliminary survey of the observations of detached solidification in space. We have successfully modeled steady state detached solidification, examined the stability of detachment, and determined the influence of buoyancy-driven convection under different conditions. Directional solidification in microgravity has often led to ingots that grew with little or no contact with the ampoule wall. When this occurred, crystallographic perfection was usually greatly improved -- often by several orders of magnitude. Indeed, under the Soviet microgravity program the major objective was to achieve detached solidification with its resulting improvement in perfection and properties. Unfortunately, until recently the true mechanisms underlying detached solidification were unknown. As a consequence, flight experiments yielded erratic results. Within the past three years, we have developed a new theoretical model that explains many of the flight results. This model gives rise to predictions of the conditions required to yield detached solidification.

Welding Behavior of Free Machining Stainless Steel

DOE Office of Scientific and Technical Information (OSTI.GOV)

BROOKS,JOHN A.; ROBINO,CHARLES V.; HEADLEY,THOMAS J.

2000-07-24

The weld solidification and cracking behavior of sulfur bearing free machining austenitic stainless steel was investigated for both gas-tungsten arc (GTA) and pulsed laser beam weld processes. The GTA weld solidification was consistent with those predicted with existing solidification diagrams and the cracking response was controlled primarily by solidification mode. The solidification behavior of the pulsed laser welds was complex, and often contained regions of primary ferrite and primary austenite solidification, although in all cases the welds were found to be completely austenite at room temperature. Electron backscattered diffraction (EBSD) pattern analysis indicated that the nature of the base metalmore » at the time of solidification plays a primary role in initial solidification. The solid state transformation of austenite to ferrite at the fusion zone boundary, and ferrite to austenite on cooling may both be massive in nature. A range of alloy compositions that exhibited good resistance to solidification cracking and was compatible with both welding processes was identified. The compositional range is bounded by laser weldability at lower Cr{sub eq}/Ni{sub eq} ratios and by the GTA weldability at higher ratios. It was found with both processes that the limiting ratios were somewhat dependent upon sulfur content.« less

Modelling Directional Solidification

NASA Technical Reports Server (NTRS)

Wilcox, William R.; Regel, Liya L.; Zhou, Jian; Yuan, Weijun

1992-01-01

The long range goal of this program has been to develop an improved understanding of phenomena of importance to directional solidification, in order to enable explanation and prediction of differences in behavior between solidification on Earth and in space. Current emphasis is on determining the influence of perturbations on directional solidification.

Laser weldability of 21Cr-6Ni-9Mn stainless steel: Part II - Weldability diagrams

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tate, Stephen B.; Javernick, Daniel Anthony; Lienert, Thomas J.

In this second part of the study, weldability diagrams developed to relate solidification crack susceptibility and chemical composition for laser welded type 21Cr-6Ni-9Mn (21-6-9) stainless steel are presented. Sigmajig testing on 14 commercial 21-6-9 alloys, 20 experimental 21-6-9 alloys, and 7 other high-N, high-Mn austenitic stainless steels was used to develop weldability diagrams for solidification crack susceptibility for laser welding of type 21-6-9. Three travel speeds were used to show the changes in minimum Cr eq/Ni eq for primary ferrite solidification as solidification rate increase d with travel speed . Primary austenite solidification was observed below 1.55 Cr eq/Ni eqmore » (Espy equivalents) at 21 mm/s travel speed. At 42 mm/s travel speed , a mix of solidification modes were displayed for alloys from 1.55-1.75 Cr eq/Ni eq. Primary ferrite solidification was observed above 1.75 Cr eq/Ni eq at both 42 and 85 mm/s travel speeds. No solidification cracking was observed for alloys with primary ferrite solidification. Lastly, variable cracking behavior was found in alloys with primary austenite solidification, but in general cracking was observed in alloys with greater than 0.02 wt-% combined impurity content according to (P+0.2S).« less

Laser weldability of 21Cr-6Ni-9Mn stainless steel: Part II - Weldability diagrams

DOE PAGES

Tate, Stephen B.; Javernick, Daniel Anthony; Lienert, Thomas J.; ...

2016-11-02

In this second part of the study, weldability diagrams developed to relate solidification crack susceptibility and chemical composition for laser welded type 21Cr-6Ni-9Mn (21-6-9) stainless steel are presented. Sigmajig testing on 14 commercial 21-6-9 alloys, 20 experimental 21-6-9 alloys, and 7 other high-N, high-Mn austenitic stainless steels was used to develop weldability diagrams for solidification crack susceptibility for laser welding of type 21-6-9. Three travel speeds were used to show the changes in minimum Cr eq/Ni eq for primary ferrite solidification as solidification rate increase d with travel speed . Primary austenite solidification was observed below 1.55 Cr eq/Ni eqmore » (Espy equivalents) at 21 mm/s travel speed. At 42 mm/s travel speed , a mix of solidification modes were displayed for alloys from 1.55-1.75 Cr eq/Ni eq. Primary ferrite solidification was observed above 1.75 Cr eq/Ni eq at both 42 and 85 mm/s travel speeds. No solidification cracking was observed for alloys with primary ferrite solidification. Lastly, variable cracking behavior was found in alloys with primary austenite solidification, but in general cracking was observed in alloys with greater than 0.02 wt-% combined impurity content according to (P+0.2S).« less

Application of perfusion culture system improves in vitro and in vivo osteogenesis of bone marrow-derived osteoblastic cells in porous ceramic materials.

PubMed

Wang, Yichao; Uemura, Toshimasa; Dong, Jian; Kojima, Hiroko; Tanaka, Junzo; Tateishi, Tetsuya

2003-12-01

Composites of bone marrow-derived osteoblasts (BMOs) and porous ceramics have been widely used as a bone graft model for bone tissue engineering. Perfusion culture has potential utility for many cell types in three-dimensional (3D) culture. Our hypothesis was that perfusion of medium would increase the cell viability and biosynthetic activity of BMOs in porous ceramic materials, which would be revealed by increased levels of alkaline phosphate (ALP) activity and osteocalcin (OCN) and enhanced bone formation in vivo. For testing in vitro, BMO/beta-tricalcium phosphate composites were cultured in a perfusion container (Minucells and Minutissue, Bad Abbach, Germany) with fresh medium delivered at a rate of 2 mL/h by a peristaltic pump. The ALP activity and OCN content of composites were measured at the end of 1, 2, 3, and 4 weeks of subculture. For testing in vivo, after subculturing for 2 weeks, the composites were subcutaneously implanted into syngeneic rats. These implants were harvested 4 or 8 weeks later. The samples then underwent a biochemical analysis of ALP activity and OCN content and were observed by light microscopy. The levels of ALP activity and OCN in the composites were significantly higher in the perfusion group than in the control group (p < 0.01), both in vitro and in vivo. Histomorphometric analysis of the hematoxylin- and eosin-stained sections revealed a higher average ratio of bone to pore in BMO/beta-TCP composites of the perfusion group after implantation: 47.64 +/- 6.16 for the perfusion group and 26.22 +/- 4.84 for control at 4 weeks (n = 6, p < 0.01); 67.97 +/- 3.58 for the perfusion group and 47.39 +/- 4.10 for control at 8 weeks (n = 6, p < 0.05). These results show that the application of a perfusion culture system during the subculture of BMOs in a porous ceramic scaffold is beneficial to their osteogenesis. After differentiation culture in vitro with the perfusion culture system, the activity of the osteoblastic cells and the consequent bone formation in vivo were significantly enhanced. These results suggest that the perfusion culture system is a valuable and convenient tool for applications in tissue engineering, especially in the generation of artificial bone tissue.

Design strategies and applications of nacre-based biomaterials.

PubMed

Gerhard, Ethan Michael; Wang, Wei; Li, Caiyan; Guo, Jinshan; Ozbolat, Ibrahim Tarik; Rahn, Kevin Michael; Armstrong, April Dawn; Xia, Jingfen; Qian, Guoying; Yang, Jian

2017-05-01

The field of tissue engineering and regenerative medicine relies heavily on materials capable of implantation without significant foreign body reactions and with the ability to promote tissue differentiation and regeneration. The field of bone tissue engineering in particular requires materials capable of providing enhanced mechanical properties and promoting osteogenic cell lineage commitment. While bone repair has long relied almost exclusively on inorganic, calcium phosphate ceramics such as hydroxyapatite and their composites or on non-degradable metals, the organically derived shell and pearl nacre generated by mollusks has emerged as a promising alternative. Nacre is a naturally occurring composite material composed of inorganic, calcium carbonate plates connected by a framework of organic molecules. Similar to mammalian bone, the highly organized microstructure of nacre endows the composite with superior mechanical properties while the organic phase contributes to significant bioactivity. Studies, both in vitro and in vivo, have demonstrated nacre's biocompatibility, biodegradability, and osteogenic potential, which are superior to pure inorganic minerals such as hydroxyapatite or non-degradable metals. Nacre can be used directly as a bulk implant or as part of a composite material when combined with polymers or other ceramics. While nacre has demonstrated its effectiveness in multiple cell culture and animal models, it remains a relatively underexplored biomaterial. This review introduces the formation, structure, and characteristics of nacre, and discusses the present and future uses of this biologically-derived material as a novel biomaterial for orthopedic and other tissue engineering applications. Mussel derived nacre, a biological composite composed of mineralized calcium carbonate platelets and interplatelet protein components, has recently gained interest as a potential alternative ceramic material in orthopedic biomaterials, combining the integration and mechanical capabilities of calcium phosphates with increased bioactivity derived from proteins and biomolecules; however, there is limited awareness of this material's potential. Herein, we present, to our knowledge, the first comprehensive review of nacre as a biomaterial. Nacre is a highly promising yet overlooked biomaterial for orthopedic tissue engineering with great potential in a wide variety of material systems. It is our hope that publication of this article will lead to increased community awareness of the potential of nacre as a versatile, bioactive ceramic capable of improving bone tissue regeneration and will elicit increased research effort and innovation utilizing nacre. Copyright © 2017 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

In vitro shear bond strength of cementing agents to fixed prosthodontic restorative materials.

PubMed

Piwowarczyk, Andree; Lauer, Hans-Christoph; Sorensen, John A

2004-09-01

Durable bonding to fixed prosthodontic restorations is desirable; however, little information is available on the strength of the bond between different cements and fixed prosthodontic restorative materials. This study determined the shear-bond strength of cementing agents to high-gold-content alloy castings and different dental ceramics: high-strength aluminum oxide (Procera AllCeram), leucite-reinforced (IPS Empress), and lithium disilicate glass-ceramic (IPS Empress 2). Prepolymerized resin composite cylinders (5.5 mm internal diameter, n=20) were bonded to the pretreated surfaces of prosthodontic materials. High-gold-content alloy and high-strength aluminum oxide surfaces were airborne-particle-abraded, and pressable ceramics were hydrofluoric acid-etched and silanized prior to cementing. The cementing agents tested were a zinc-phosphate cement (Fleck's zinc cement), glass ionomer cements (Fuji I, Ketac-Cem), resin-modified glass ionomer cements (Fuji Plus, Fuji Cem, RelyX Luting), resin cements (RelyX ARC, Panavia F, Variolink II, Compolute), and a self-adhesive universal resin cement (RelyX Unicem). Half the specimens (n=10) were tested after 30 minutes; the other half (n=10) were stored in distilled water at 37 degrees C for 14 days and then thermal cycled 1000 times between 5 degrees C and 55 degrees C prior to testing. Shear-bond strength tests were performed using a universal testing machine at a constant crosshead speed of 0.5 mm/min. Statistical analysis was performed by multifactorial analysis of variance taking interactions between effects into account. For multiple paired comparisons, the Tukey method was used (alpha=.05). In a 3-way ANOVA model, the main factors substrate, cement, time, and all corresponding interactions were statistically significant (all P <.0001). In subsequent separate 1-way or 2-way ANOVA models for each substrate type, significant differences between cement types and polymerizing modes were found (all P <.001). None of the cement types provided the highest bonding values with all substrate types. After 14 days of water storage followed by thermal cycling, only the self-adhesive universal resin cement (RelyX Unicem) and 2 of the resin cements (Panavia F and Compolute) exhibited strong bond strengths to specific prosthodontic materials. In contrast, zinc-phosphate, glass ionomer, and resin-modified glass ionomer cements showed the lowest values of all tested cementing agents after 14 days of water storage followed by thermal cycling.

Solidification Sequence of Spray-Formed Steels

NASA Astrophysics Data System (ADS)

Zepon, Guilherme; Ellendt, Nils; Uhlenwinkel, Volker; Bolfarini, Claudemiro

2016-02-01

Solidification in spray-forming is still an open discussion in the atomization and deposition area. This paper proposes a solidification model based on the equilibrium solidification path of alloys. The main assumptions of the model are that the deposition zone temperature must be above the alloy's solidus temperature and that the equilibrium liquid fraction at this temperature is reached, which involves partial remelting and/or redissolution of completely solidified droplets. When the deposition zone is cooled, solidification of the remaining liquid takes place under near equilibrium conditions. Scanning electron microscopy (SEM) and optical microscopy (OM) were used to analyze the microstructures of two different spray-formed steel grades: (1) boron modified supermartensitic stainless steel (SMSS) and (2) D2 tool steel. The microstructures were analyzed to determine the sequence of phase formation during solidification. In both cases, the solidification model proposed was validated.

Study of structural, electrical, and dielectric properties of phosphate-borate glasses and glass-ceramics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Melo, B. M. G.; Graça, M. P. F., E-mail: mpfg@ua.pt; Prezas, P. R.

2016-08-07

In this work, phosphate-borate based glasses with molar composition 20.7P{sub 2}O{sub 5}–17.2Nb{sub 2}O{sub 5}–13.8WO{sub 3}–34.5A{sub 2}O–13.8B{sub 2}O{sub 3}, where A = Li, Na, and K, were prepared by the melt quenching technique. The as-prepared glasses were heat-treated in air at 800 °C for 4 h, which led to the formation of glass-ceramics. These high chemical and thermal stability glasses are good candidates for several applications such as fast ionic conductors, semiconductors, photonic materials, electrolytes, hermetic seals, rare-earth ion host solid lasers, and biomedical materials. The present work endorses the analysis of the electrical conductivity of the as-grown samples, and also the electrical, dielectric,more » and structural changes established by the heat-treatment process. The structure of the samples was analyzed using X-Ray powder Diffraction (XRD), Raman spectroscopy, and density measurements. Both XRD and Raman analysis confirmed crystals formation through the heat-treatment process. The electrical ac and dc conductivities, σ{sub ac} and σ{sub dc}, respectively, and impedance spectroscopy measurements as function of the temperature, varying from 200 to 380 K, were investigated for the as-grown and heat-treated samples. The impedance spectroscopy was measured in the frequency range of 100 Hz–1 MHz.« less

Microsphere-Based Scaffolds Encapsulating Tricalcium Phosphate And Hydroxyapatite For Bone Regeneration

PubMed Central

Gupta, Vineet; Lyne, Dina V.; Barragan, Marilyn; Berkland, Cory J.; Detamore, Michael S.

2016-01-01

Bioceramic mixtures of tricalcium phosphate (TCP) and hydroxyapatite (HAp) are widely used for bone regeneration because of their excellent cytocompatibility, osteoconduction, and osteoinduction. Therefore, we hypothesized that incorporation of a mixture of TCP and HAp in microsphere-based scaffolds would enhance osteogenesis of rat bone marrow stromal cells (rBMSCs) compared to a positive control of scaffolds with encapsulated bone-morphogenic protein-2 (BMP-2). Poly(D,L-lactic-co-glycolic acid) (PLGA) microsphere-based scaffolds encapsulating TCP and HAp mixtures in two different ratios (7:3 and 1:1) were fabricated with the same net ceramic content (30 wt%) to evaluate how incorporation of these ceramic mixtures would affect the osteogenesis in rBMSCs. Encapsulation of TCP/HAp mixtures impacted microsphere morphologies and the compressive moduli of the scaffolds. Additionally, TCP/HAp mixtures enhanced the end-point secretion of extracellular matrix (ECM) components relevant to bone tissue compared to the “blank” (PLGA-only) microsphere-based scaffolds as evidenced by the biochemical, gene expression, histology, and immunohistochemical characterization. Moreover, the TCP/HAp mixture groups even surpassed the BMP-2 positive control group in some instances in terms of matrix synthesis and gene expression. Lastly, gene expression data suggested that the rBMSCs responded differently to different TCP/HAp ratios presented to them. Altogether, it can be concluded that TCP/HAp mixtures stimulated the differentiation of rBMSCs toward an osteoblastic phenotype, and therefore may be beneficial in gradient microsphere-based scaffolds for osteochondral regeneration. PMID:27272903

Kinetics of dissolution of thorium and uranium doped britholite ceramics

NASA Astrophysics Data System (ADS)

Dacheux, N.; Du Fou de Kerdaniel, E.; Clavier, N.; Podor, R.; Aupiais, J.; Szenknect, S.

2010-09-01

In the field of immobilization of actinides in phosphate-based ceramics, several thorium and uranium doped britholite samples were submitted to leaching tests. The normalized dissolution rates determined for several pH values, temperatures and acidic media from the calcium release range from 4.7 × 10 -2 g m -2 d -1 to 21.6 g m -2 d -1. Their comparison with that determined for phosphorus, thorium and uranium revealed that the dissolution is clearly incongruent for all the conditions examined. Whatever the leaching solution considered, calcium and phosphorus elements were always released with higher RL values than the other elements (Nd, Th, U). Simultaneously, thorium was found to quickly precipitate as alteration product, leading to diffusion phenomena for uranium. For all the media considered, the uranium release is higher than that of thorium, probably due to its oxidation from tetravalent oxidation state to uranyl. Moreover, the evaluation of the partial order related to proton concentration and the apparent energy of activation suggest that the reaction of dissolution is probably controlled by surface chemical reactions occurring at the solid/liquid interface. Finally, comparative leaching tests performed in sulphuric acid solutions revealed a significant influence of such media on the chemical durability of the leached pellets, leading to higher normalized dissolution rates for all the elements considered. On the basis of the results of chemical speciation, this difference was mainly explained in the light of higher complexion constants by sulfate ions compared to nitrate, chloride and phosphate.

Initial deposition of calcium phosphate ceramic on polystyrene and polytetrafluoroethylene by rf magnetron sputtering deposition

NASA Astrophysics Data System (ADS)

Feddes, B.; Wolke, J. G. C.; Jansen, J. A.; Vredenberg, A. M.

2003-03-01

Calcium phosphate (CaP) coatings can be applied to improve the biological performance of polymeric medical implants. A strong interfacial bond between ceramic and polymer is required for clinical applications. Because the chemical structure of an interface plays an important role in the adhesion of a coating, we studied the formation of the interface between CaP and polystyrene (PS) and polytetrafluoroethylene (PTFE). The coating was deposited in a radio frequency (rf) magnetron sputtering deposition system. Prior to the deposition, some samples received an oxygen plasma pretreatment. We found that the two substrates show a strongly different reactivity towards CaP. On PS a phosphorus and oxygen enrichment is present at the interface. This is understood from POx complexes that are able to bind to the PS. The effects of the plasma pretreatment are overruled by the deposition process itself. On PTFE, a calcium enrichment and an absence of phosphorus is found at the interface. The former is the result of CaF2-like material being formed at the interface. The latter may be the result of phosphorus reacting with escaping fluorine to a PF3 molecule, which than escapes from the material as a gas molecule. We found that the final structure of the interface is mostly controlled by the bombardment of energetic particles escaping either from the plasma or from the sputtering target. The work described here can be used to understand and improve the adhesion of CaP coatings deposited on medical substrates.

Experiment/facility requirements document for the Space Station Furnace Facility. Section 1: Integrated configuration

NASA Astrophysics Data System (ADS)

1992-05-01

The function of the Space Station Furnace Facility (SSFF) is to support materials research into the crystal growth and solidification processes of electronic and photonic materials, metals and alloys, and glasses and ceramics. To support this broad base of research requirements, the SSFF will employ a variety of furnace modules which will be operated, regulated, and supported by a core of common subsystems. Furnace modules may be reconfigured or specifically developed to provide unique solidification conditions for each set of experiments. The SSFF modular approach permits the addition of new or scaled-up furnace modules to support the evolution of the facility as new science requirements are identified. The SSFF Core is of modular design to permit augmentation for enhanced capabilities. The fully integrated configuration of the SSFF will consist of three racks with the capability of supporting up to two furnace modules per rack. The initial configuration of the SSFF will consist of two of the three racks and one furnace module. This Experiment/Facility Requirements Document (E/FRD) describes the integrated facility requirements for the Space Station Freedom (SSF) Integrated Configuration-1 (IC1) mission. The IC1 SSFF will consist of two racks: the Core Rack, with the centralized subsystem equipment; and the Experiment Rack-1, with Furnace Module-1 and the distributed subsystem equipment to support the furnace. The SSFF support functions are provided by the following Core subsystems: power conditioning and distribution subsystem (SSFF PCDS); data management subsystem (SSFF DMS); thermal control Subsystem (SSFF TCS); gas distribution subsystem (SSFF GDS); and mechanical structures subsystem (SSFF MSS).

Formation of Y(x)Nd(1-x) Ba2Cu3O(7-delta) (0 = or < x < or = 0.7) Superconductors from an Undercooled Melt Via Aero-Acoustic Levitation

NASA Technical Reports Server (NTRS)

Gustafson, D. E.; Hofmeister, W. H.; Bayuzick, R. J.

2001-01-01

Melt processing of RE123 superconductors has gained importance in recent years. While the first high temperature superconductors (HTSCs) were made using traditional ceramic press and sinter technology, recent fabrication efforts have employed alternate processing techniques including laser ablation and ion beam assisted deposition for thin film fabrication of tapes and wires and melt growth for bulk materials. To optimize these techniques and identify other potential processing strategies, phase relation studies on HTSCs have been conducted on a wide variety of superconducting compounds using numerous processing strategies. This data has enhanced the understanding of these complex systems and allowed more accurate modeling of phase interactions. All of this research has proved useful in identifying processing capabilities for HTSCs but has failed to achieve a breakthrough for wide spread application of these materials. This study examines the role of full to partial substitution of Nd in the Y123 structure under rapid solidification conditions. Aero-acoustic levitation (AAL) was used to levitate and undercool RE123 in pure oxygen binary alloys with RE = Nd an Y along a range of compositions corresponding to Y(x)Nd(1-x) Ba2Cu3O(7-delta) (0 = or < x < or = 0.7) which were melted by a CO2 laser. Higher Y content spheres could not be melted in the AAL and were excluded from this report. Solidification structures were examined using scanning electron microscopy, electron dispersive spectroscopy, and powder x-ray diffraction to characterize microstructures and identify phases.

Experiment/facility requirements document for the Space Station Furnace Facility. Section 1: Integrated configuration

NASA Technical Reports Server (NTRS)

1992-01-01

The function of the Space Station Furnace Facility (SSFF) is to support materials research into the crystal growth and solidification processes of electronic and photonic materials, metals and alloys, and glasses and ceramics. To support this broad base of research requirements, the SSFF will employ a variety of furnace modules which will be operated, regulated, and supported by a core of common subsystems. Furnace modules may be reconfigured or specifically developed to provide unique solidification conditions for each set of experiments. The SSFF modular approach permits the addition of new or scaled-up furnace modules to support the evolution of the facility as new science requirements are identified. The SSFF Core is of modular design to permit augmentation for enhanced capabilities. The fully integrated configuration of the SSFF will consist of three racks with the capability of supporting up to two furnace modules per rack. The initial configuration of the SSFF will consist of two of the three racks and one furnace module. This Experiment/Facility Requirements Document (E/FRD) describes the integrated facility requirements for the Space Station Freedom (SSF) Integrated Configuration-1 (IC1) mission. The IC1 SSFF will consist of two racks: the Core Rack, with the centralized subsystem equipment; and the Experiment Rack-1, with Furnace Module-1 and the distributed subsystem equipment to support the furnace. The SSFF support functions are provided by the following Core subsystems: power conditioning and distribution subsystem (SSFF PCDS); data management subsystem (SSFF DMS); thermal control Subsystem (SSFF TCS); gas distribution subsystem (SSFF GDS); and mechanical structures subsystem (SSFF MSS).

Dissolution and precipitation behaviors of silicon-containing ceramic coating on Mg-Zn-Ca alloy in simulated body fluid.

PubMed

Pan, Yaokun; Chen, Chuanzhong; Wang, Diangang; Huang, Danlan

2014-10-01

We prepared Si-containing and Si-free coatings on Mg-1.74Zn-0.55Ca alloy by micro-arc oxidation. The dissolution and precipitation behaviors of Si-containing coating in simulated body fluid (SBF) were discussed. Corrosion products were characterized by scanning electron microscope (SEM), X-ray diffractometer (XRD), fourier transform infrared spectrometer (FT-IR) and X-ray photoelectron spectrometer (XPS). Electrochemical workstation, inductively coupled plasma atomic emission spectrometer (ICP-AES), flame atomic absorption spectrophotometer (AAS) and pH meter were employed to detect variations of electrochemical parameter and ions concentration respectively. Results indicate that the fast formation of calcium phosphates is closely related to the SiOx(n-) groups, which induce the heterogeneous nucleation of amorphous hydroxyapatite (HA) by sorption of calcium and phosphate ions. Copyright © 2014 Elsevier B.V. All rights reserved.

Method for preparing hydrous zirconium oxide gels and spherules

DOEpatents

Collins, Jack L.

2003-08-05

Methods for preparing hydrous zirconium oxide spherules, hydrous zirconium oxide gels such as gel slabs, films, capillary and electrophoresis gels, zirconium monohydrogen phosphate spherules, hydrous zirconium oxide spherules having suspendable particles homogeneously embedded within to form a composite sorbent, zirconium monohydrogen phosphate spherules having suspendable particles of at least one different sorbent homogeneously embedded within to form a composite sorbent having a desired crystallinity, zirconium oxide spherules having suspendable particles homogeneously embedded within to form a composite, hydrous zirconium oxide fiber materials, zirconium oxide fiber materials, hydrous zirconium oxide fiber materials having suspendable particles homogeneously embedded within to form a composite, zirconium oxide fiber materials having suspendable particles homogeneously embedded within to form a composite and spherules of barium zirconate. The hydrous zirconium oxide spherules and gel forms prepared by the gel-sphere, internal gelation process are useful as inorganic ion exchangers, catalysts, getters and ceramics.

Healing of extraction sockets filled with BoneCeramic® prior to implant placement: preliminary histological findings.

PubMed

De Coster, Peter; Browaeys, Hilde; De Bruyn, Hugo

2011-03-01

Various grafting materials have been designed to minimize edentulous ridge volume loss following tooth extraction by encouraging new bone formation in healing sockets. BoneCeramic® is a composite of hydroxyapatite and bèta-tricalcium phosphate with pores of 100-500 microns. The aim of this study was to evaluate bone regeneration in healing sockets substituted with BoneCeramic® prior to implant procedures. Fifteen extraction sockets were substituted with BoneCeramic® and 14 sockets were left to heal naturally in 10 patients (mean age 59.6 years). Biopsies were collected only from the implant recipient sites during surgery after healing periods ranging from 6-74 weeks (mean 22). In total, 24 biopsies were available; 10 from substituted and 14 from naturally healed sites. In one site, the implant was not placed intentionally and, in four substituted sites, implant placement had to be postponed due to inappropriate healing, hence from five sites biopsies were not available. Histological sections were examined by transmitted light microscope. At the time of implant surgery, bone at substituted sites was softer than in controls, compromising initial implant stability. New bone formation at substituted sites was consistently poorer than in controls, presenting predominantly loose connective tissue and less woven bone. The use of BoneCeramic® as a grafting material in fresh extraction sockets appears to interfere with normal healing processes of the alveolar bone. On the basis of the present preliminary findings, its indication as a material for bone augmentation, when implant placement is considered within 6-38 weeks after extraction, should be revised. © 2009, Copyright the Authors. Journal Compilation © 2011, Wiley Periodicals, Inc.

Casting And Solidification Technology (CAST): Directional solidification phenomena in a metal model at reduced gravity

NASA Technical Reports Server (NTRS)

Mccay, M. H.

1988-01-01

The Casting and Solidification Technology (CAST) experiment will study the phenomena that occur during directional solidification of an alloy, e.g., constitutional supercooling, freckling, and dendrite coarsening. The reduced gravity environment of space will permit the individual phenomena to be examined with minimum complication from buoyancy driven flows.

Simulation Computation of 430 Ferritic Stainless Steel Solidification

NASA Astrophysics Data System (ADS)

Pang, Ruipeng; Li, Changrong; Wang, Fuming; Hu, Lifu

The solidification structure of 430 ferritic stainless steel has been calculated in the solidification process by using 3D-CAFE model under the condition of water cooling. The calculated results consistent with those obtained from experiment. Under watercooling condition, the solidification structure consists of chilled layer, columnar grain zone, transition zone and equiaxed grain zone.

A comparative study of proliferation and osteogenic differentiation of adipose-derived stem cells on akermanite and beta-TCP ceramics.

PubMed

Liu, Qihai; Cen, Lian; Yin, Shuo; Chen, Lei; Liu, Guangpeng; Chang, Jiang; Cui, Lei

2008-12-01

This study investigated the in vitro effects of akermanite, a new kind of Ca-, Mg-, Si-containing bioceramic, on the attachment, proliferation and osteogenic differentiation of human adipose-derived stem cells (hASCs). Parallel comparison of the cellular behaviors of hASCs on the akermanite was made with those on beta-tricalcium phosphate (beta-TCP). Scanning electron microscope (SEM) observation and fluorescent DiO labeling were carried out to reveal the attachment and growth of hASCs on the two ceramic surfaces, while the quantitative assay of cell proliferation with time was detected by DNA assay. Osteogenic differentiation of hASCs cultured on the akermanite and beta-TCP was assayed by ALP expression and osteocalcin (OCN) deposition, which was further confirmed by Real-time PCR analysis for markers of osteogenic differentiation. It was shown that hASCs attached and spread well on the akermanite as those on beta-TCP, and similar proliferation behaviors of hASCs were observed on the two ceramics. Both of them exhibited good compatibility to hASCs with only minor cytotoxicity as compared with the tissue culture plates. Interestingly, the osteogenic differentiation of hASCs could be enhanced on the akermanite compared with that on the beta-TCP when the culture time was extended to approximately 10 days. Thus, it can be ascertained that akermanite ceramics may serve as a potential scaffold for bone tissue engineering.

Development of a double-layered ceramic filter for aerosol filtration at high-temperatures: the filter collection efficiency.

PubMed

de Freitas, Normanda L; Gonçalves, José A S; Innocentini, Murilo D M; Coury, José R

2006-08-25

The performance of double-layered ceramic filters for aerosol filtration at high temperatures was evaluated in this work. The filtering structure was composed of two layers: a thin granular membrane deposited on a reticulate ceramic support of high porosity. The goal was to minimize the high pressure drop inherent of granular structures, without decreasing their high collection efficiency for small particles. The reticulate support was developed using the technique of ceramic replication of polyurethane foam substrates of 45 and 75 pores per inch (ppi). The filtering membrane was prepared by depositing a thin layer of granular alumina-clay paste on one face of the support. Filters had their permeability and fractional collection efficiency analyzed for filtration of an airborne suspension of phosphatic rock in temperatures ranging from ambient to 700 degrees C. Results revealed that collection efficiency decreased with gas temperature and was enhanced with filtration time. Also, the support layer influenced the collection efficiency: the 75 ppi support was more effective than the 45 ppi. Particle collection efficiency dropped considerably for particles below 2 microm in diameter. The maximum collection occurred for particle diameters of approximately 3 microm, and decreased again for diameters between 4 and 8 microm. Such trend was successfully represented by the proposed correlation, which is based on the classical mechanisms acting on particle collection. Inertial impaction seems to be the predominant collection mechanism, with particle bouncing/re-entrainment acting as detachment mechanisms.

Retention of metal-ceramic crowns with contemporary dental cements.

PubMed

Johnson, Glen H; Lepe, Xavier; Zhang, Hai; Wataha, John C

2009-09-01

New types of crown and bridge cement are in use by practitioners, and independent studies are needed to assess their effectiveness. The authors conducted a study in three parts (study A, study B, and study C) and to determine how well these new cements retain metal-ceramic crowns. The authors prepared teeth with a 20-degree taper and a 4-millimeter length. They cast high-noble metal-ceramic copings, then fitted and cemented them with a force of 196 newtons. The types of cements they used were zinc phosphate, resin-modified glass ionomer, conventional resin and self-adhesive modified resin. They thermally cycled the cemented copings, then removed them. They recorded the removal force and calculated the stress of dislodgment by using the surface area of each preparation. They used a single-factor analysis of variance to analyze the data (alpha = .05). The mean stresses necessary to remove crowns, in megapascals, were 8.0 for RelyX Luting (3M ESPE, St. Paul, Minn.), 7.3 for RelyX Unicem (3M ESPE), 5.7 for Panavia F (Kuraray America, New York) and 4.0 for Fuji Plus (GC America, Alsip, Ill.) in study A; 8.1 for RelyX Luting, 2.6 for RelyX Luting Plus (3M ESPE) and 2.8 for Fuji CEM (GC America) in study B; and 4.9 for Maxcem (Kerr, Orange, Calif.), 4.0 for BisCem (Bisco, Schaumburg, Ill.), 3.7 for RelyX Unicem Clicker (3M ESPE), 2.9 for iCEM (Heraeus Kulzer, Armonk, N.Y.) and 2.3 for Fleck's Zinc Cement (Keystone Industries, Cherry Hill, N.J.) in study C. Powder-liquid versions of new cements were significantly more retentive than were paste-paste versions of the same cements. The mean value of crown removal stress for the new self-adhesive modified-resin cements varied appreciably among the four cements tested. All cements retained castings as well as or better than did zinc phosphate cement. Powder-liquid versions of cements, although less convenient to mix, may be a better clinical choice when crown retention is an issue. All cements tested will retain castings adequately on ideal preparations because the corresponding removal stresses are comparable with or higher than those associated with zinc phosphate. Powder-liquid resin-modified glass ionomer cement, selected self-adhesive modified-resin cements and conventional resin cements provide additional retention when desired.

High strength, biodegradable and cytocompatible alpha tricalcium phosphate-iron composites for temporal reduction of bone fractures.

PubMed

Montufar, E B; Casas-Luna, M; Horynová, M; Tkachenko, S; Fohlerová, Z; Diaz-de-la-Torre, S; Dvořák, K; Čelko, L; Kaiser, J

2018-04-01

In this work alpha tricalcium phosphate (α-TCP)/iron (Fe) composites were developed as a new family of biodegradable, load-bearing and cytocompatible materials. The composites with composition from pure ceramic to pure metallic samples were consolidated by pulsed electric current assisted sintering to minimise processing time and temperature while improving their mechanical performance. The mechanical strength of the composites was increased and controlled with the Fe content, passing from brittle to ductile failure. In particular, the addition of 25 vol% of Fe produced a ceramic matrix composite with elastic modulus much closer to cortical bone than that of titanium or biodegradable magnesium alloys and specific compressive strength above that of stainless steel, chromium-cobalt alloys and pure titanium, currently used in clinic for internal fracture fixation. All the composites studied exhibited higher degradation rate than their individual components, presenting values around 200 μm/year, but also their compressive strength did not show a significant reduction in the period required for bone fracture consolidation. Composites showed preferential degradation of α-TCP areas rather than β-TCP areas, suggesting that α-TCP can produce composites with higher degradation rate. The composites were cytocompatible both in indirect and direct contact with bone cells. Osteoblast-like cells attached and spread on the surface of the composites, presenting proliferation rate similar to cells on tissue culture-grade polystyrene and they showed alkaline phosphatase activity. Therefore, this new family of composites is a potential alternative to produce implants for temporal reduction of bone fractures. Biodegradable alpha-tricalcium phosphate/iron (α-TCP/Fe) composites are promising candidates for the fabrication of temporal osteosynthesis devices. Similar to biodegradable metals, these composites can avoid implant removal after bone fracture healing, particularly in young patients. In this work, α-TCP/Fe composites are studied for the first time in a wide range of compositions, showing not only higher degradation rate in vitro than pure components, but also good cytocompatibility and mechanical properties controllable with the Fe content. Ceramic matrix composites show high specific strength and low elastic modulus, thus better fulfilling the requirements for bone fractures fixation. A significant advance over previous works on the topic is the use of pulsed electric current assisted sintering together with α-TCP, convenient to improve the mechanical performance and degradation rate, respectively. Copyright © 2018 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Preparation and Characterization of a Calcium Phosphate Ceramic for the Immobilization of Chloride-containing Intermediate Level Waste

DOE Office of Scientific and Technical Information (OSTI.GOV)

Metcalfe, Brian; Donald, Ian W.; Scheele, Randall D.

2003-12-01

Attention has recently been given to the immobilization of special categories of radioactive wastes, some of which contain high concentrations of actinide chlorides. Although vitrification in phosphate glass has been proposed, this was rejected because of the high losses of chloride. On the basis of non-radioactive and, more recently, radioactive studies, we have shown that calcium phosphate is an effective host for immobilizing the chloride constituents [1]. In this instance, the chlorine is retained as chloride, rather than evolved as a chlorine-bearing gas. The immobilized product is in the form of a free-flowing, non-hygroscopic powder, in which the chlorides aremore » chemically combined within the mineral phases chlorapatite [Ca5(PO4)3Cl] and spodiosite [Ca2(PO4)Cl]. Data from studies on non-radioactive simulated waste consisting of a mixture of CaCl2 and SmCl3, and radioactive simulated waste composed of CaCl2 with PuCl3 or PuCl3 and AmCl3, are presented and compared. The XRD data confirm the presence of chlorapatite and spodiosite in the non-radioactive and radioactive materials. The durability of all specimens was measured with a modified MCC-1 test. Releases of Cl after 28 days were 1.6 x 10-3 g m-2 for the non-radioactive specimens and 7 x 10-3 g m-2 for the Pu-bearing specimens. Releases of Ca after 28 days were 0.3 x 10-3 and 2.0 x 10-3 g m-2 for the non-radioactive composition and the Pu composition, respectively, whilst release of Pu from the radioactive specimens was lower for the mixed Pu/Am specimen at 1.2 x 10-5g m-2. The release of Am from the mixed Pu/Am composition was exceptionally low at 2.4 x 10-7 g m-2. Overall, the release rate data suggest that the ceramics dissolve congruently, followed by precipitation of Sm, Pu and Am as less soluble phases, possibly oxides or phosphates. The differences in behaviour noted between non-radioactive and radioactive specimens are interpreted in terms of the crystal chemistry of the individual systems.« less

Development and Characterization of Biphasic Hydroxyapatite/β-TCP Cements

PubMed Central

Gallinetti, Sara; Canal, Cristina; Ginebra, Maria-Pau; Ferreira, J

2014-01-01

Biphasic calcium phosphate bioceramics composed of hydroxyapatite (HA) and β-tricalcium phosphate (β-TCP) have relevant properties as synthetic bone grafts, such as tunable resorption, bioactivity, and intrinsic osteoinduction. However, they have some limitations associated to their condition of high-temperature ceramics. In this work self-setting Biphasic Calcium Phosphate Cements (BCPCs) with different HA/β-TCP ratios were obtained from self-setting α-TCP/β-TCP pastes. The strategy used allowed synthesizing BCPCs with modulated composition, compressive strength, and specific surface area. Due to its higher solubility, α-TCP was fully hydrolyzed to a calcium-deficient HA (CDHA), whereas β-TCP remained unreacted and completely embedded in the CDHA matrix. Increasing amounts of the non-reacting β-TCP phase resulted in a linear decrease of the compressive strength, in association to the decreasing amount of precipitated HA crystals, which are responsible for the mechanical consolidation of apatitic cements. Ca2+ release and degradation in acidic medium was similar in all the BCPCs within the timeframe studied, although differences might be expected in longer term studies once β-TCP, the more soluble phase was exposed to the surrounding media. PMID:25866411

Comparison of low-shear and high-shear granulation processes: effect on implantable calcium phosphate granule properties.

PubMed

Chevalier, E; Viana, M; Cazalbou, S; Chulia, D

2009-10-01

Calcium phosphate porous ceramics present a great interest not only as complex bone defect fillers but also as drug delivery systems. Most of the methods described in the literature to fabricate pellets are based on compaction, casting into spherical molds, or on processes such as liquid immiscibility or foaming. Despite wet granulation is used in a wide range of applications in pharmaceuticals, food, detergents, fertilizers, and minerals, it is not applied in the biomaterial field to produce granules. In this study physicochemical and in vitro drug delivery properties of implantable calcium phosphate granules, produced by two wet agglomeration processes, were compared. Pellets obtained by high shear granulation (granulation in a Mi-Pro apparatus) were shown to be more spherical and less friable than granules elaborated by low shear process (granulation in a Kenwood apparatus). Although Mi-Pro pellets had a slightly lower porosity compared to Kenwood granules, ibuprofen loading efficiency and dissolution profiles were not statistically different and the release mechanism was mainly controlled by diffusion, in both cases. Mi-Pro pellets appeared to be better candidates as bone defect fillers and local drug delivery systems as far as they were more spherical and less friable than Kenwood agglomerates.

Hydrophobic and Metallophobic Surfaces: Highly Stable Non-wetting Inorganic Surfaces Based on Lanthanum Phosphate Nanorods

PubMed Central

Sankar, Sasidharan; Nair, Balagopal N.; Suzuki, Takehiro; Anilkumar, Gopinathan M.; Padmanabhan, Moothetty; Hareesh, Unnikrishnan Nair S.; Warrier, Krishna G.

2016-01-01

Metal oxides, in general, are known to exhibit significant wettability towards water molecules because of the high feasibility of synergetic hydrogen-bonding interactions possible at the solid-water interface. Here we show that the nano sized phosphates of rare earth materials (Rare Earth Phosphates, REPs), LaPO4 in particular, exhibit without any chemical modification, unique combination of intrinsic properties including remarkable hydrophobicity that could be retained even after exposure to extreme temperatures and harsh hydrothermal conditions. Transparent nanocoatings of LaPO4 as well as mixture of other REPs on glass surfaces are shown to display notable hydrophobicity with water contact angle (WCA) value of 120° while sintered and polished monoliths manifested WCA greater than 105°. Significantly, these materials in the form of coatings and monoliths also exhibit complete non-wettability and inertness towards molten metals like Ag, Zn, and Al well above their melting points. These properties, coupled with their excellent chemical and thermal stability, ease of processing, machinability and their versatile photo-physical and emission properties, render LaPO4 and other REP ceramics utility in diverse applications. PMID:26955962

Cu2+, Co2+ and Cr3+ doping of a calcium phosphate cement influences materials properties and response of human mesenchymal stromal cells.

PubMed

Schamel, Martha; Bernhardt, Anne; Quade, Mandy; Würkner, Claudia; Gbureck, Uwe; Moseke, Claus; Gelinsky, Michael; Lode, Anja

2017-04-01

The application of biologically active metal ions to stimulate cellular reactions is a promising strategy to accelerate bone defect healing. Brushite-forming calcium phosphate cements were modified with low doses of Cu 2+ , Co 2+ and Cr 3+ . The modified cements released the metal ions in vitro in concentrations which were shown to be non-toxic for cells. The release kinetics correlated with the solubility of the respective metal phosphates: 17-45 wt.-% of Co 2+ and Cu 2+ , but <1 wt.-% of Cr 3+ were released within 28days. Moreover, metal ion doping led to alterations in the exchange of calcium and phosphate ions with cell culture medium. In case of cements modified with 50mmol Cr 3+ /mol β-tricalcium phosphate (β-TCP), XRD and SEM analyses revealed a significant amount of monetite and a changed morphology of the cement matrix. Cell culture experiments with human mesenchymal stromal cells indicated that the observed cell response is not only influenced by the released metal ions but also by changed cement properties. A positive effect of modifications with 50mmol Cr 3+ or 10mmol Cu 2+ per mol β-TCP on cell behaviour was observed in indirect and direct culture. Modification with Co 2+ resulted in a clear suppression of cell proliferation and osteogenic differentiation. In conclusion, metal ion doping of the cement influences cellular activities in addition to the effect of released metal ions by changing properties of the ceramic matrix. Copyright © 2016 Elsevier B.V. All rights reserved.

Mesoporous nitrogen-doped carbon-glass ceramic cathodes for solid-state lithium-oxygen batteries.

PubMed

Kichambare, Padmakar; Rodrigues, Stanley; Kumar, Jitendra

2012-01-01

The composite of nitrogen-doped carbon (N-C) blend with lithium aluminum germanium phosphate (LAGP) was studied as cathode material in a solid-state lithium-oxygen cell. Composite electrodes exhibit high electrochemical activity toward oxygen reduction. Compared to the cell capacity of N-C blend cathode, N-C/LAGP composite cathode exhibits six times higher discharge cell capacity. A significant enhancement in cell capacity is attributed to higher electrocatalytic activity and fast lithium ion conduction ability of LAGP in the cathode. © 2011 American Chemical Society

Advanced Zinc Phosphate Conversion and Pre-Ceramic Polymetallosiloxane Coatings for Corrosion Protection of Steel and Aluminum, and Characteristics of Polyphenyletheretherketone-Based Materials

DTIC Science & Technology

1992-09-24

which the trivalent ion is the principal oxidation state, preferentially reacts with hydroxylated organosilane to form the Al-O-Si linkage at a low... tig front the carboxylic acid, COOH, in the p(AA) [6j. The spectra for all of the cobalt- and nickel-incorporated Zn-Ph samples show a slight...to study bonding in chromium , manganese, iron, and cobalt compounds J Chem Phys 57 (1972) pp 973-982 1 1 Lindberg, B.J. et at. Molecular

Solidification/Stabilization Resource Guide

EPA Pesticide Factsheets

This Solidification/Stabilization Resource Guide is intended to inform site cleanup managers of recently-published materials such as field reports and guidance documents that address issues relevant to solidification/stabilization technologies.

The Solidification of Multicomponent Alloys

PubMed Central

Boettinger, William J.

2017-01-01

Various topics taken from the author’s research portfolio that involve multicomponent alloy solidification are reviewed. Topics include: ternary eutectic solidification and Scheil-Gulliver paths in ternary systems. A case study of the solidification of commercial 2219 aluminum alloy is described. Also described are modifications of the Scheil-Gulliver analysis to treat dendrite tip kinetics and solid diffusion for multicomponent alloys. PMID:28819348

X-ray imaging and controlled solidification of Al-Cu alloys toward microstructures by design

DOE PAGES

Clarke, Amy J.; Tourret, Damien; Imhoff, Seth D.; ...

2015-01-30

X-ray imaging, which permits the microscopic visualization of metal alloy solidification dynamics, can be coupled with controlled solidification to create microstructures by design. In this study, this x-ray image shows a process-derived composite microstructure being made from a eutectic Al-17.1 at.%Cu alloy by successive solidification and remelting steps.

Strength reliability and in vitro degradation of three-dimensional powder printed strontium-substituted magnesium phosphate scaffolds.

PubMed

Meininger, Susanne; Mandal, Sourav; Kumar, Alok; Groll, Jürgen; Basu, Bikramjit; Gbureck, Uwe

2016-02-01

Strontium ions (Sr(2+)) are known to prevent osteoporosis and also encourage bone formation. Such twin requirements have motivated researchers to develop Sr-substituted biomaterials for orthopaedic applications. The present study demonstrates a new concept of developing Sr-substituted Mg3(PO4)2 - based biodegradable scaffolds. In particular, this work reports the fabrication, mechanical properties with an emphasis on strength reliability as well as in vitro degradation of highly biodegradable strontium-incorporated magnesium phosphate cements. These implantable scaffolds were fabricated using three-dimensional powder printing, followed by high temperature sintering and/or chemical conversion, a technique adaptable to develop patient-specific implants. A moderate combination of strength properties of 36.7MPa (compression), 24.2MPa (bending) and 10.7MPa (tension) were measured. A reasonably modest Weibull modulus of up to 8.8 was recorded after uniaxial compression or diametral tensile tests on 3D printed scaffolds. A comparison among scaffolds with varying compositions or among sintered or chemically hardened scaffolds reveals that the strength reliability is not compromised in Sr-substituted scaffolds compared to baseline Mg3(PO4)2. The micro-computed tomography analysis reveals the presence of highly interconnected porous architecture in three-dimension with lognormal pore size distribution having median in the range of 17.74-26.29μm for the investigated scaffolds. The results of extensive in vitro ion release study revealed passive degradation with a reduced Mg(2+) release and slow but sustained release of Sr(2+) from strontium-substituted magnesium phosphate scaffolds. Taken together, the present study unequivocally illustrates that the newly designed Sr-substituted magnesium phosphate scaffolds with good strength reliability could be used for biomedical applications requiring consistent Sr(2+)- release, while the scaffold degrades in physiological medium. The study investigates the additive manufacturing of scaffolds based on different strontium-substituted magnesium phosphate bone cements by means of three-dimensional powder printing technique (3DPP). Magnesium phosphates were chosen due to their higher biodegradability compared to calcium phosphates, which is due to both a higher solubility as well as the absence of phase changes (to low soluble hydroxyapatite) in vivo. Since strontium ions are known to promote bone formation by stimulating osteoblast growth, we aimed to establish such a highly degradable magnesium phosphate ceramic with an enhanced bioactivity for new bone ingrowth. After post-processing, mechanical strengths of up to 36.7MPa (compression), 24.2MPa (bending) and 10.7MPa (tension) could be achieved. Simultaneously, the failure reliability of those bioceramic implant materials, measured by Weibull modulus calculations, were in the range of 4.3-8.8. Passive dissolution studies in vitro proved an ion release of Mg(2+) and PO4(3-) as well as Sr(2+), which is fundamental for in vivo degradation and a bone growth promoting effect. In our opinion, this work broadens the range of bioceramic bone replacement materials suitable for additive manufacturing processing. The high biodegradability of MPC ceramics together with the anticipated promoting effect on osseointegration opens up the way for a patient-specific treatment with the prospect of a fast and complete healing of bone fractures. Copyright © 2015 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Parabolic aircraft solidification experiments

NASA Technical Reports Server (NTRS)

Workman, Gary L. (Principal Investigator); Smith, Guy A.; OBrien, Susan

1996-01-01

A number of solidification experiments have been utilized throughout the Materials Processing in Space Program to provide an experimental environment which minimizes variables in solidification experiments. Two techniques of interest are directional solidification and isothermal casting. Because of the wide-spread use of these experimental techniques in space-based research, several MSAD experiments have been manifested for space flight. In addition to the microstructural analysis for interpretation of the experimental results from previous work with parabolic flights, it has become apparent that a better understanding of the phenomena occurring during solidification can be better understood if direct visualization of the solidification interface were possible. Our university has performed in several experimental studies such as this in recent years. The most recent was in visualizing the effect of convective flow phenomena on the KC-135 and prior to that were several successive contracts to perform directional solidification and isothermal casting experiments on the KC-135. Included in this work was the modification and utilization of the Convective Flow Analyzer (CFA), the Aircraft Isothermal Casting Furnace (ICF), and the Three-Zone Directional Solidification Furnace. These studies have contributed heavily to the mission of the Microgravity Science and Applications' Materials Science Program.

Solidification kinetics of a Cu-Zr alloy: ground-based and microgravity experiments

NASA Astrophysics Data System (ADS)

Galenko, P. K.; Hanke, R.; Paul, P.; Koch, S.; Rettenmayr, M.; Gegner, J.; Herlach, D. M.; Dreier, W.; Kharanzhevski, E. V.

2017-04-01

Experimental and theoretical results obtained in the MULTIPHAS-project (ESA-European Space Agency and DLR-German Aerospace Center) are critically discussed regarding solidification kinetics of congruently melting and glass forming Cu50Zr50 alloy samples. The samples are investigated during solidification using a containerless technique in the Electromagnetic Levitation Facility [1]. Applying elaborated methodologies for ground-based and microgravity experimental investigations [2], the kinetics of primary dendritic solidification is quantitatively evaluated. Electromagnetic Levitator in microgravity (parabolic flights and on board of the International Space Station) and Electrostatic Levitator on Ground are employed. The solidification kinetics is determined using a high-speed camera and applying two evaluation methods: “Frame by Frame” (FFM) and “First Frame - Last Frame” (FLM). In the theoretical interpretation of the solidification experiments, special attention is given to the behavior of the cluster structure in Cu50Zr50 samples with the increase of undercooling. Experimental results on solidification kinetics are interpreted using a theoretical model of diffusion controlled dendrite growth.

Study of Solidification Cracking in a Transformation-Induced Plasticity-Aided Steel

NASA Astrophysics Data System (ADS)

Agarwal, G.; Kumar, A.; Gao, H.; Amirthalingam, M.; Moon, S. C.; Dippenaar, R. J.; Richardson, I. M.; Hermans, M. J. M.

2018-04-01

In situ high-temperature laser scanning confocal microscopy is applied to study solidification cracking in a TRIP steel. Solidification cracking was observed in the interdendritic region during the last stage of solidification. Atom probe tomography revealed notable enrichment of phosphorus in the last remaining liquid. Phase field simulations also confirm phosphorus enrichment leading to severe undercooling of more than 160 K in the interdendritic region. In the presence of tensile stress, an opening at the interdendritic region is difficult to fill with the remaining liquid due to low permeability and high viscosity, resulting in solidification cracking.

Microstructural development during solidification of stainless steel alloys

NASA Astrophysics Data System (ADS)

Elmer, J. W.; Allen, S. M.; Eagar, T. W.

1989-10-01

The microstructures that develop during the solidification of stainless steel alloys are related to the solidification conditions and the specific alloy composition. The solidification conditions are determined by the processing method, i.e., casting, welding, or rapid solidification, and by parametric variations within each of these techniques. One variable that has been used to characterize the effects of different processing conditions is the cooling rate. This factor and the chemical composition of the alloy both influence (1) the primary mode of solidification, (2) solute redistribution and second-phase formation during solidification, and (3) the nucleation and growth behavior of the ferrite-to-austenite phase transformation during cooling. Consequently, the residual ferrite content and the microstructural morphology depend on the cooling rate and are governed by the solidification process. This paper investigates the influence of cooling rate on the microstructure of stainless steel alloys and describes the conditions that lead to the many microstructural morphologies that develop during solidification. Experiments were performed on a series of seven high-purity Fe-Ni-Cr alloys that spanned the line of twofold saturation along the 59 wt pct Fe isopleth of the ternary alloy system. High-speed electron-beam surface-glazing was used to melt and resolidify these alloys at scan speeds up to 5 m/s. The resulting cooling rates were shown to vary from 7°C/s to 7.5×106°C/s, and the resolidified melts were analyzed by optical metallographic methods. Five primary modes of solidification and 12 microstructural morphologies were characterized in the resolidified alloys, and these features appear to be a complete “set” of the possible microstructures for 300-series stainless steel alloys. The results of this study were used to create electron-beam scan speed vs composition diagrams, which can be used to predict the primary mode of solidification and the microstructural morphology for different processing conditions. Furthermore, changes in the primary solidification mode were observed in alloys that lie on the chromium-rich side of the line of twofold saturation when they are cooled at high rates. These changes were explained by the presence of metastable austenite, which grows epitaxially and can dominate the solidification microstructure throughout the resolidified zone at high cooling rates.

Design of Natural Hydroxyapatite as bio-composite ceramics (HAP): Experimental and Numerical Study

NASA Astrophysics Data System (ADS)

Belghazi, Z.; Katundi, D.; Ayari, F.; Bayraktar, E.

2011-01-01

Hydroxyapatite (HAP—Ca10(PO4)6 (OH)2), which exhibits excellent biocompatibility in the body, is one of the most widely used bioactive ceramics for biomedical applications. Along with the ability to carry the load, one of the most important properties of materials used for bone replacement is biocompatibility. In fact, HAP is a bioactive material and it can incorporate into bone structures, supporting bone in-growth without breaking down or dissolving, and it interacts with the living tissue due to the presence of free calcium and phosphate compounds. Generally, Al2O3 powder is added to HAP powder in order to obtain high fracture toughness. Al2O3 has good mechanical properties as compared with HAP, and exhibits extremely high stability with human tissues [1-6]. In this paper, the effect of microwave sintering temperature on the relative density, hardness, and phase purity of compacted bovine Hydroxyapatite (BHA) powder was reported. This research is a comprehensive attempt to develop Hydroxyapatite bio composite ceramics reinforced with alumina—Al2O3, pure titanium and pure pulverised boron powder. A Finite Element (FEM) analysis is also used for modelling to simulate the macroscopic behaviour of this material, taking into account the relevant microscopic scales.

Effect of pH values on surface modification and solubility of phosphate bioglass-ceramics in the CaO-P 2O 5-Na 2O-SrO-ZnO system

NASA Astrophysics Data System (ADS)

Li, Xudong; Cai, Shu; Zhang, Wenjuang; Xu, Guohua; Zhou, Wei

2009-08-01

The bioactive glass-ceramics in the CaO-P 2O 5-Na 2O-SrO-ZnO system were synthesized by the sol-gel technique, and then chemically treated at different pH values to study the solubility and surface modification. Samples sintered at 650 °C for 4 h consisted of the crystalline phase β-Ca 2P 2O 7 and the glass matrix. After soaking in the solution at pH 1.0, the residual glass matrix on the surface appeared entirely dissolved and no new phase could be detected. Whereas at pH 3.0, web-like layer exhibiting peaks corresponding to CaP 2O 6 was formed and covered the entire surface of the sample. When conducted at pH 10.0, only part of the glass matrix was dissolved and a new phase Ca 4P 6O 19 was precipitated, forming the petaline layer. The chemical treatment can easily change the surface morphologies and phase composition of this bioactive glass-ceramics. The higher level of surface roughness resulting from the new-formed layer would improve the interface bonding and benefit for cell adhesion.

Analysis and calculation of macrosegregation in a casting ingot. MPS solidification model. Volume 3: Operating manual

NASA Technical Reports Server (NTRS)

Maples, A. L.

1980-01-01

The operation of solidification model 1 is described. Model 1 calculates the macrosegregation in a rectangular ingot of a binary alloy as a result of horizontal axisymmetric bidirectional solidification. The calculation is restricted to steady-state solidification; there is no variation in final local average composition in the direction of isotherm movement. The physics of the model are given.

X-Ray Transmission Microscope Development

NASA Technical Reports Server (NTRS)

Kaukler, William F.

1997-01-01

We have succeeded in meeting the goals set out in the proposal. A cadre of detector technologies is available to suit the requirements of the experiment. Resolutions of both real-time and absolute limits to resolution exceed the initial aspirations. Obtaining sufficient contrast is still a significant limitation but can be overcome by Judicious selection of the specimen composition. This can only take time and trial and error for a successful result. The 4th generation furnace provides the capability of real-time in-situ observations of composite alloy development. A low detection sensitivity however, has still made it difficult to observe dendritic growth, although it has been 'seen' in raw video; it was not a recordable signal. We have examined flight ampoules with XTM to observe particle and thermocouple placement, crucible flaws and cracks in collaboration with the Particle Pushing and Engulfment flight experiment (Dr. Stefanescu, UA, P.I.). The value of an in flight XTM to guard against experiment failure and safety assurance is obvious. Although not attributable to equipment limitations, a quest to observe particle pushing was not successful. We tried at length to prepare specimens that would demonstrate particle pushing. Instead, we were successful in imaging the interface deformation due to the thermal field distortion of a ceramic particle or void and to compare to calculated shapes. In theory, we should have been able to make major inroads to this field if the particles could be pushed and the velocities adjusted to make critical measurements. On the other hand, critical issues of sample preparation for the PEP flight experiment were established, particularly the clustering of particles and trapped voids. In this regard, the XTM did prove very useful so that flight specimens would work as expected and to perform post flight analysis. Although not a clear result, particle pushing of precipitates was observed in an Al-Si-Mn alloy. It may be that to be pushed, the particles need to be small and have clean surfaces like one might obtain from in-situ precipitation. The ability to image features in real time skill enable more fundamental and detailed understanding of solidification dynamics in microgravity than had previously been possible, thus, allowing the full benefits of microgravity experiments be applied towards rigorous testing of critical solidification models. The XTM is also a valuable tool for post solidification metallography. The 3-dimensional distribution of solute and solidification features within the specimen volume can be viewed without sectioning or other treatment when the solute has sufficiently higher atomic mass than the solvent. Thus the XTM could provide the first practical method for on orbit microstructural (metallographic) analysis by the astronauts or by telescience.

DEMONSTRATION BULLETIN: SOLIDIFICATION/STABILIZATION PROCESS, Hazcon, Inc.

EPA Science Inventory

The solidification/stabilization technology mixes hazardous wastes, cement, water and an additive called Chloranan. Chloranan, a nontoxic chemical, encapsulates organic molecules, rendering them ineffective in retarding or inhibiting solidification. This treatment technol...

Investigating gas-phase defect formation in late-stage solidification using a novel phase-field crystal alloy model

NASA Astrophysics Data System (ADS)

Wang, Nan; Smith, Nathan; Provatas, Nikolas

2017-09-01

We study late-stage solidification and the associated formation of defects in alloy materials using a novel model based on the phase-field-crystal technique. It is shown that our model successfully captures several important physical phenomena that occur in the late stages of solidification, including solidification shrinkage, liquid cavitation and microsegregation, all in a single framework. By examining the interplay of solidification shrinkage and solute segregation, this model reveals that the formation of gas pore defects at the late stage of solidification can lead to nucleation of second phase solid particles due to solute enrichment in the eutectic liquid driven by gas-phase nucleation and growth. We also predict a modification of the Gulliver-Scheil equation in the presence of gas pockets in confined liquid pools.

Core solidification and dynamo evolution in a mantle-stripped planetesimal

NASA Astrophysics Data System (ADS)

Scheinberg, A.; Elkins-Tanton, L. T.; Schubert, G.; Bercovici, D.

2016-01-01

The physical processes active during the crystallization of a low-pressure, low-gravity planetesimal core are poorly understood but have implications for asteroidal magnetic fields and large-scale asteroidal structure. We consider a core with only a thin silicate shell, which could be analogous to some M-type asteroids including Psyche, and use a parameterized thermal model to predict a solidification timeline and the resulting chemical profile upon complete solidification. We then explore the potential strength and longevity of a dynamo in the planetesimal's early history. We find that cumulate inner core solidification would be capable of sustaining a dynamo during solidification, but less power would be available for a dynamo in an inward dendritic solidification scenario. We also model and suggest limits on crystal settling and compaction of a possible cumulate inner core.

Size-dependent microstructures in rapidly solidified uranium-niobium powder particles

DOE PAGES

McKeown, Joseph T.; Hsiung, Luke L.; Park, Jong M.; ...

2016-06-14

The microstructures of rapidly solidified U-6wt%Nb powder particles synthesized by centrifugal atomization were characterized using scanning electron microscopy and transmission electron microscopy. Observed variations in microstructure are related to particle sizes. All of the powder particles exhibited a two-zone microstructure. The formation of this two-zone microstructure is described by a transition from solidification controlled by internal heat flow and high solidification rate during recalescence (micro-segregation-free or partitionless growth) to solidification controlled by external heat flow with slower solidification rates (dendritic growth with solute redistribution). The extent of partitionless solidification increased with decreasing particle size due to larger undercoolings in smallermore » particles prior to solidification. The metastable phases that formed are related to variations in Nb concentration across the particles. Lastly, the microstructures of the powders were heavily twinned.« less

Evaluation of the onset of failure under mechanical and thermal stresses on luting agent for metal–ceramic and metal crowns by finite element analysis

PubMed Central

Agnihotri, Hema; Bhatnagar, Naresh; Rao, G. Venugopal; Jain, Veena; Parkash, Hari; Kar, Aswini Kumar

2010-01-01

Long-term clinical failures of cemented prosthesis depend, to a large extent, on the integrity of the luting agent. The causative factors that lead to microfracture and, hence, failure of the luting agents are the stresses acting inside the oral cavity. Therefore, the present study was designed to develop an understanding of the relationship between stresses in the tooth and the failure potential of the luting agent. Two-dimensional finite element stress analysis was performed on the mandibular second premolar. The behavior of zinc-phosphate and glass-ionomer were studied under different crowns (metal–ceramic and metal crown) and loading conditions (mechanical force of 450 N acting vertically over the occlusal surface, thermal loads of 60° and 0°C). It was observed from the study that failure threshold of the luting agent was influenced both by the elastic modulus of the luting agent and by the type of the crown. PMID:22114426

A two-scale Weibull approach to the failure of porous ceramic structures made by robocasting: possibilities and limits

PubMed Central

Genet, Martin; Houmard, Manuel; Eslava, Salvador; Saiz, Eduardo; Tomsia, Antoni P.

2012-01-01

This paper introduces our approach to modeling the mechanical behavior of cellular ceramics, through the example of calcium phosphate scaffolds made by robocasting for bone-tissue engineering. The Weibull theory is used to deal with the scaffolds’ constitutive rods statistical failure, and the Sanchez-Palencia theory of periodic homogenization is used to link the rod- and scaffold-scales. Uniaxial compression of scaffolds and three-point bending of rods were performed to calibrate and validate the model. If calibration based on rod-scale data leads to over-conservative predictions of scaffold’s properties (as rods’ successive failures are not taken into account), we show that, for a given rod diameter, calibration based on scaffold-scale data leads to very satisfactory predictions for a wide range of rod spacing, i.e. of scaffold porosity, as well as for different loading conditions. This work establishes the proposed model as a reliable tool for understanding and optimizing cellular ceramics’ mechanical properties. PMID:23439936

Effect of bleaching agent and topical fluoride application on color and gloss of dental ceramics.

PubMed

Pires-de-Souza, Fernanda de Carvalho Panzeri; Contente, Marta Maria Martins Giamatei; Alandia-Román, Carla Cecilia; Vicente, Sergio Augusto de Freitas; Tonani, Rafaella

2016-01-01

The aim of this study was to evaluate the effect of 16% carbamide peroxide and 1.23% acidulated phosphate fluoride application and their association with a change in color (ΔE*) and brightness of dental ceramic submitted to different finishing procedures. A total of 120 test specimens were fabricated and randomly divided into 3 groups (n = 40) according to the type of finishing: glazing; polishing; or polishing and glazing. Initial color and brightness readouts were taken, and the finished specimens were divided into groups (n = 10) according to the treatment to which they were submitted: fluoride; bleaching; bleaching and fluoride; or control. After this, final color and brightness readouts were taken. The type of polishing had no influence on ΔE* or brightness (P > 0.05). Regardless of which solution was used, a decrease in brightness occurred only for the group treated with bleach and fluoride (P < 0.05). The results showed the use of fluoride after bleaching may interfere with the esthetics of a restoration.

Directional Solidification and Liquidus Projection of the Sn-Co-Cu System

NASA Astrophysics Data System (ADS)

Chen, Sinn-Wen; Chang, Jui-Shen; Pan, Kevin; Hsu, Chia-Ming; Hsu, Che-Wei

2013-04-01

This study investigates the Sn-Co-Cu ternary system, which is of interest to the electronics industry. Ternary Sn-Co-Cu alloys were prepared, their as-solidified microstructures were examined, and their primary solidification phases were determined. The primary solidification phases observed were Cu, Co, Co3Sn2, CoSn, CoSn2, Cu6Sn5, Co3Sn2, γ, and β phases. Although there are ternary compounds reported in this ternary system, no ternary compound was found as the primary solidification phase. The directional solidification technique was applied when difficulties were encountered using the conventional quenching method to distinguish the primary solidification phases, such as Cu6Sn5, Cu3Sn, and γ phases. Of all the primary solidification phases, the Co3Sn2 and Co phases have the largest compositional regimes in which alloys display them as the primary solidification phases. There are four class II reactions and four class III reactions. The reactions with the highest and lowest reaction temperatures are both class III reactions, and are L + CoSn2 + Cu6Sn5 = CoSn3 at 621.5 K (348.3 °C) and L + Co3Sn2 + CoSn = Cu6Sn5 at 1157.8 K (884.6 °C), respectively.

Early-term and mid-term histologic events during single-level posterolateral intertransverse process fusion with rhBMP-2/collagen carrier and a ceramic bulking agent in a nonhuman primate model: implications for bone graft preparation.

PubMed

Khan, Safdar N; Toth, Jeffrey M; Gupta, Kavita; Glassman, Steven D; Gupta, Munish C

2014-06-01

We used a nonhuman primate lumbar intertransverse process arthrodesis model to evaluate biological cascade of bone formation using different carrier preparation methods with a single dose of recombinant human bone morphogenetic protein-2 (rhBMP-2) at early time points. To examine early-term/mid-term descriptive histologic and computerized tomographic events in single-level uninstrumented posterolateral nonhuman primate spinal fusions using rhBMP-2/absorbable collagen sponge (ACS) combined with ceramic bulking agents in 3 different configurations. rhBMP-2 on an ACS carrier alone leads to consistent posterolateral lumbar spine fusions in lower-order animals; however, these results have been difficult to replicate in nonhuman primates. Twelve skeletally mature, rhesus macaque monkeys underwent single-level posterolateral arthrodesis at L4-L5. A hydroxyapatite/β-tricalcium phosphate ceramic bulking agent in 3 formulations was used in the treatment groups (n=3). When used, rhBMP-2/ACS at 1.5 mg/cm (3.0 mg rhBMP-2) was combined with 2.5 cm of ceramic bulking agent per side. Animals were euthanized at 4 and 12 weeks postoperative. Computerized tomography scans were performed immediately postoperatively and every 4 weeks until they were euthanized. Sagittal histologic sections were evaluated for bone histogenesis and location, cellular infiltration of the graft/substitute, and bone remodeling activity. Significant histologic differences in the developing fusion appeared between the 3 rhBMP-2/ACS treatment groups at 4 and 12 weeks. At 4 weeks, bone formation appeared to originate at the transverse process and the intertransverse membrane. Cellular infiltration was greatest in granular ceramic groups compared with matrix ceramic group. Minimal to no residual ACS was identified at the early time point. At 12 weeks, marked ceramic remodeling was observed with continued bone formation noted in all carrier groups. At the early time period, histology showed that bone formation appeared to originate at the transverse processes and the intertransverse membrane, indicating that the dorsal muscle bed may not be the only location for bone formation. Histology also showed that the collagen carrier for rhBMP-2 is mostly resorbed by 4 weeks. Our results and previous literature indicate that ceramic bulking agents are needed to provide resistance to compression caused by paraspinal muscles on the fusion bed in the posterolateral environment. Histology showed that ceramic bulking agents may offer long-term scaffolding and a structure to supporting bone formation of the developing fusion mass.

Rapid Solidification in Bulk Ti-Nb Alloys by Single-Track Laser Melting

NASA Astrophysics Data System (ADS)

Roehling, John D.; Perron, Aurélien; Fattebert, Jean-Luc; Haxhimali, Tomorr; Guss, Gabe; Li, Tian T.; Bober, David; Stokes, Adam W.; Clarke, Amy J.; Turchi, Patrice E. A.; Matthews, Manyalibo J.; McKeown, Joseph T.

2018-05-01

Single-track laser melting experiments were performed on bulk Ti-Nb alloys to explore process parameters and the resultant macroscopic structure and microstructure. The microstructures in Ti-20Nb and Ti-50Nb (at.%) alloys exhibited cellular growth during rapid solidification, with average cell size of approximately 0.5 µm. Solidification velocities during cellular growth were calculated from images of melt tracks. Measurements of the composition in the cellular and intercellular regions revealed nonequilibrium partitioning and its dependence on velocity during rapid solidification. Experimental results were used to benchmark a phase-field model to describe rapid solidification under conditions relevant to additive manufacturing.

Evolutions of lamellar structure during melting and solidification of Fe9577 nanoparticle from molecular dynamics simulations

NASA Astrophysics Data System (ADS)

Wu, Yongquan; Shen, Tong; Lu, Xionggang

2013-03-01

A structural evolution during solidification and melting processes of nanoparticle Fe9577 was investigated from MD simulations. A perfect lamellar structure, consisting alternately of fcc and hcp layers, was obtained from solidification process. A structural heredity of early embryo is proposed to explain the structural preference of solidification. Defects were found inside the solid core and play the same role as surface premelting on melting. hcp was found more stable than fcc in high temperature. The difference between melting and solidification points can be deduced coming fully from the overcoming of thermodynamic energy barrier, instead of kinetic delay of structural relaxation.

The Solidification Velocity of Undercooled Nickel and Titanium Alloys with Dilute Solute

NASA Technical Reports Server (NTRS)

Algoso, Paul R.; Altgilbers, A. S.; Hofmeister, William H.; Bayuzick, Robert J.

2003-01-01

The study of solidification velocity is important for two reasons. First, understanding the manner in which the degree of undercooling of the liquid and solidification velocity affect the microstructure of the solid is fundamental. Second, there is disagreement between theoretical predictions of the relationship between undercooling and solidification velocity and experimental results. Thus, the objective of this research is to accurately and systematically quantify the solidification velocity as a function of undercooling for dilute nickel-and titanium-based alloys. The alloys chosen for study cover a wide range of equilibrium partition coefficients, and the results are compared to current theory.

Development of a High Chromium Ni-Base Filler Metal Resistant to Ductility Dip Cracking and Solidification Cracking

NASA Astrophysics Data System (ADS)

Hope, Adam T.

Many nuclear reactor components previously constructed with Ni-based alloys containing 20 wt% Cr have been found to be susceptible to stress corrosion cracking. The nuclear power industry now uses high chromium (˜30wt%) Ni-based filler metals to mitigate stress corrosion cracking. Current alloys are plagued with weldability issues, either solidification cracking or ductility dip cracking (DDC). Solidification cracking is related to solidification temperature range and the DDC is related to the fraction eutectic present in the microstructure. It was determined that an optimal alloy should have a solidification temperature range less than 150°C and at least 2% volume fraction eutectic. Due to the nature of the Nb rich eutectic that forms, it is difficult to avoid both cracking types simultaneously. Through computational modeling, alternative eutectic forming elements, Hf and Ta, have been identified as replacements for Nb in such alloys. Compositions have been optimized through a combination of computational and experimental techniques combined with a design of experiment methodology. Small buttons were melted using commercially pure materials in a copper hearth to obtain the desired compositions. These buttons were then subjected to a gas tungsten arc spot weld. A type C thermocouple was used to acquire the cooling history during the solidification process. The cooling curves were processed using Single Sensor Differential Thermal Analysis to determine the solidification temperature range, and indicator of solidification cracking susceptibility. Metallography was performed to determine the fraction eutectic present, an indicator of DDC resistance. The optimal level of Hf to resist cracking was found to be 0.25 wt%. The optimal level of Ta was found to be 4 wt%. gamma/MC type eutectics were found to form first in all Nb, Ta, and Hf-bearing compositions. Depending on Fe and Cr content, gamma/Laves eutectic was sometimes found in Nb and Ta-bearing compositions, while Hf-bearing compositions had gamma/Ni7Hf2 as the final eutectic to solidify. This study found that the extra Cr in the current generation alloys promotes the gamma/Laves phase eutectic, which expands the solidification temperature range and promotes solidification cracking. Both Ta-bearing and Hf-bearing eutectics were found to solidify at higher temperatures than Nb-bearing eutectics, leading to narrower solidification temperature ranges. Weldability testing on the optimized Ta-bearing compositions revealed good resistance to both DDC and solidification cracking. Unexpectedly, the optimized Hf-bearing compositions were quite susceptible to solidification cracking. This led to an investigation on the possible wetting effect of eutectics on solidification cracking susceptibly, and a theory on how wetting affects the solidification crack susceptibility and the volume fraction of eutectic needed for crack healing has been proposed. Alloys with eutectics that easily wet the grain boundaries have increased solidification crack susceptibility at low volume fraction eutectics, but as the fraction eutectic is increased, experience crack healing at relatively lower fraction eutectics than alloys with eutectics that don't wet as easily. Hf rich eutectics were found to wet grain boundaries significantly more than Nb rich eutectics. Additions of Mo were also found to increase the wetting of eutectics in Nb-bearing alloys.

Repair of Cranial Bone Defects Using rhBMP2 and Submicron Particle of Biphasic Calcium Phosphate Ceramics with Through-Hole

PubMed Central

Jeong, Byung-Chul; Choi, Hyuck; Hur, Sung-Woong; Kim, Jung-Woo; Oh, Sin-Hye; Kim, Hyun-Seung; Song, Soo-Chang; Lee, Keun-Bae; Park, Kwang-Bum; Koh, Jeong-Tae

2015-01-01

Recently a submicron particle of biphasic calcium phosphate ceramic (BCP) with through-hole (donut-shaped BCP (d-BCP)) was developed for improving the osteoconductivity. This study was performed to examine the usefulness of d-BCP for the delivery of osteoinductive rhBMP2 and the effectiveness on cranial bone regeneration. The d-BCP was soaked in rhBMP2 solution and then freeze-dried. Scanning electron microscope (SEM), energy dispersive spectroscopy (EDS), and Raman spectroscopy analyses confirmed that rhBMP2 was well delivered onto the d-BCP surface and the through-hole. The bioactivity of the rhBMP2/d-BCP composite was validated in MC3T3-E1 cells as an in vitro model and in critical-sized cranial defects in C57BL/6 mice. When freeze-dried d-BCPs with rhBMP2 were placed in transwell inserts and suspended above MC3T3-E1, alkaline phosphatase activity and osteoblast-specific gene expression were increased compared to non-rhBMP2-containing d-BCPs. For evaluating in vivo effectiveness, freeze-dried d-BCPs with or without rhBMP2 were implanted into critical-sized cranial defects. Microcomputed tomography and histologic analysis showed that rhBMP2-containing d-BCPs significantly enhanced cranial bone regeneration compared to non-rhBMP2-containing control. These results suggest that a combination of d-BCP and rhBMP2 can accelerate bone regeneration, and this could be used to develop therapeutic strategies in hard tissue healing. PMID:26491693

Repair of Cranial Bone Defects Using rhBMP2 and Submicron Particle of Biphasic Calcium Phosphate Ceramics with Through-Hole.

PubMed

Jeong, Byung-Chul; Choi, Hyuck; Hur, Sung-Woong; Kim, Jung-Woo; Oh, Sin-Hye; Kim, Hyun-Seung; Song, Soo-Chang; Lee, Keun-Bae; Park, Kwang-Bum; Koh, Jeong-Tae

2015-01-01

Recently a submicron particle of biphasic calcium phosphate ceramic (BCP) with through-hole (donut-shaped BCP (d-BCP)) was developed for improving the osteoconductivity. This study was performed to examine the usefulness of d-BCP for the delivery of osteoinductive rhBMP2 and the effectiveness on cranial bone regeneration. The d-BCP was soaked in rhBMP2 solution and then freeze-dried. Scanning electron microscope (SEM), energy dispersive spectroscopy (EDS), and Raman spectroscopy analyses confirmed that rhBMP2 was well delivered onto the d-BCP surface and the through-hole. The bioactivity of the rhBMP2/d-BCP composite was validated in MC3T3-E1 cells as an in vitro model and in critical-sized cranial defects in C57BL/6 mice. When freeze-dried d-BCPs with rhBMP2 were placed in transwell inserts and suspended above MC3T3-E1, alkaline phosphatase activity and osteoblast-specific gene expression were increased compared to non-rhBMP2-containing d-BCPs. For evaluating in vivo effectiveness, freeze-dried d-BCPs with or without rhBMP2 were implanted into critical-sized cranial defects. Microcomputed tomography and histologic analysis showed that rhBMP2-containing d-BCPs significantly enhanced cranial bone regeneration compared to non-rhBMP2-containing control. These results suggest that a combination of d-BCP and rhBMP2 can accelerate bone regeneration, and this could be used to develop therapeutic strategies in hard tissue healing.

LIBS analysis of hydroxyapatite extracted from bovine bone for Ca/P ratio measurements

NASA Astrophysics Data System (ADS)

Tariq, Usman; Haider, Zuhaib; Hussain, Rafaqat; Tufail, Kashif; Ali, Jalil

2017-03-01

Hydroxyapatite has been extensively used as a potential biocompatible ceramic in many orhtopedic applications. Hydroxyapatite is one of the members of calcium phosphate family and been used extensively as a bone substitute. The mechanical properties of hydroxyapatite itself, ceramics and bone cements prepared from hydroxyapatite vary greatly with slight variation in its Ca/P ratio. At present EDX, XRD, XRF and ICP-OES are being used for the determination of Ca/P ratio in hydroxyapatite. These techniques require special sample preparation, may also use toxic chemicals and usually are not very fast in giving the measurements. We report LIBS as a rapid alternative technique for calculation of Ca/P ratio in hydroxyapatite extracted from bovine bone (BHA). Ca/P ratio in laboratory prepared HA is calculated using LIBS and the results are validated against EDX results Ca/P ratio of the hydroxyapatite was calculated as 1.54±0.19 using LIBS while 1.63±0.03 using EDX. Ca/P ratio calculated by LIBS and EDX and showed comparable results with a difference of 5.5%. Moreover, plasma temperature and the ratio of the calcium (ion) line to calcium (atomic) line did not show significant variation in plasma conditions during measurements. The present study has demonstrated that LIBS can also be used for the determination of Ca/P ratio of hydroxyapatite and other calcium phosphates. At the request of all authors of the paper, and with the agreement of the Proceedings Editor, an updated version of this article was published on 24 May 2017.

Heterotopic bone formation in the musculus latissimus dorsi of sheep using β-tricalcium phosphate scaffolds: evaluation of an extended prefabrication time on bone formation and matrix degeneration.

PubMed

Spalthoff, S; Jehn, P; Zimmerer, R; Möllmann, U; Gellrich, N-C; Kokemueller, H

2015-06-01

We previously generated viable heterotopic bone in living animals and found that 3 months of intrinsic vascularization improved bone formation and matrix degeneration. In this study, we varied the pre-vascularization time to determine its effects on the kinetics of bone formation and ceramic degradation. Two 25-mm-long cylindrical β-tricalcium phosphate scaffolds were filled intraoperatively with autogenous iliac crest bone marrow and implanted in the latissimus dorsi muscle in six sheep. To examine the effect of axial perfusion, one scaffold was surgically implanted with (group C) or without (group D) a central vascular bundle. All animals were sacrificed 6 months postoperatively and histomorphometric measurements were compared to previous results. All implanted scaffolds exhibited ectopic bone growth. However, bone growth was not significantly different between the 3-month (group A, 0.191±0.097 vs. group C, 0.237±0.075; P=0.345) and 6-month (group B, 0.303±0.105 vs. group D, 0.365±0.258; P=0.549) pre-vascularization durations, regardless of vessel supply; early differences between surgically and extrinsically vascularized constructs disappeared after 6 months. Here, we describe a reliable procedure for generating ectopic bone in vivo. A 3-month pre-vascularization duration appears sufficient and ceramic degradation proceeds in accordance with bone generation, supporting the hypothesis of cell-mediated resorption. Copyright © 2014 International Association of Oral and Maxillofacial Surgeons. Published by Elsevier Ltd. All rights reserved.

Fracture rates of IPS Empress all-ceramic crowns--a systematic review.

PubMed

Heintze, Siegward D; Rousson, Valentin

2010-01-01

The aim of this study was to evaluate the clinical fracture rate of crowns fabricated with the pressable, leucite-reinforced ceramic IPS Empress, and relate the results to the type of tooth restored. The database SCOPUS was searched for clinical studies involving full-coverage crowns made of IPS Empress. To assess the fracture rate of the crowns in relation to the type of restored tooth and study, Poisson regression analysis was used. Seven clinical studies were identified involving 1,487 adhesively luted crowns (mean observation time: 4.5+/-1.7 years) and 81 crowns cemented with zinc-phosphate cement (mean observation time: 1.6+/-0.8 years). Fifty-seven of the adhesively luted crowns fractured (3.8%). The majority of fractures (62%) occurred between the third and sixth year after placement. There was no significant influence regarding the test center on fracture rate, but the restored tooth type played a significant role. The hazard rate (per year) for crowns was estimated to be 5 in every 1,000 crowns for incisors, 7 in every 1,000 crowns for premolars, 12 in every 1,000 crowns for canines, and 16 in every 1,000 crowns for molars. One molar crown in the zinc-phosphate group fractured after 1.2 years. Adhesively luted IPS Empress crowns showed a low fracture rate for incisors and premolars and a somewhat higher rate for molars and canines. The sample size of the conventionally luted crowns was too small and the observation period too short to draw meaningful conclusions.

Efficacy of Bone Source™ and Cementek™ in comparison with Endobon™ in critical size metaphyseal defects, using a minipig model.

PubMed

Spies, Christian K G; Schnürer, Stefan; Gotterbarm, Tobias; Breusch, Steffen J

2010-01-01

To examine and compare biocompatibility, osteocompatibility, rate of resorption, and remodelling dynamics of 2 calcium phosphate cements in comparison with a well-established hydroxyapatite ceramic. In a randomised fashion, Bone Source™, Cementek™, and Endobon™ were implanted bilaterally into the proximal metaphyseal tibiae of 35 Göttinger minipigs in a direct right vs. left intra-individual comparison. Fluorescent labelling was used. Histological and morphometric evaluations were carried out at 6, 12, and 52 weeks. All bone substitutes showed good biocompatibility, bioactivity, and osteoconductivity. Endobon™ was not degraded over the follow-up period. Cementek™ was degraded constantly and significantly over the time intervals, whereas Bone Source™ was degraded mainly from the 6 week to 12 week interval. After 52 weeks, a significant difference of residual material within the defect zone was detected between all substitutes, with the highest resorption rate for Cementek™. Bone Source™ was least degraded. Defects filled with Endobon™ were characterised by a significantly continuous bony ingrowth over the time intervals. Bone formation within the defects filled with Cementek™ and Bone Source™ showed significant peaks 12 weeks after implantation. After 52 weeks, a significant difference in the amount of new bone within the defect area was detected, with the highest levels for Endobon™, followed by Cementek™. After 1 year a restitution ad integrum could not be observed in any treatment group. The ceramic Endobon™ showed the expected response histologically. Based on its porosity it excelled in osteoconductivity. Concerning the calcium phosphate cements, a thorough osseous incorporation seemed to inhibit further degradation of both bone substitute materials.

Analytical Solution for the Critical Velocity of Pushing/Engulfment Transition

NASA Technical Reports Server (NTRS)

Catalina, Adrian V.; Stefanescu, Doru M.; Sen, Subhayu

2004-01-01

The distribution of ceramic particles in a metal matrix composite material depends primarily on the interaction of the particles with the solid/liquid interface during the solidification process. A numerical model that describes the evolution of the shape of the solid/liquid interface in the proximity of a foreign particle will presented in this paper. The model accounts for the influence of the temperature gradient and the Gibbs-Thomson and disjoining pressure effects. It shows that for the systems characterized by k(sub p) < k(sub L) the disjoining pressure causes the interface curvature to change its sign in the close-contact particle/interface region. It also shows that the increase of the temperature gradient diminishes the effect of the disjoining pressure. The analysis of the numerical results obtained for a large range of processing conditions and materials parameters has led to the development of an analytical solution for the critical velocity of pushing/engulfinent transition. The theoretical results will be discussed and compared with the experimental measurements performed under microgravity conditions.

Numerical Modeling of Fiber-Reinforced Metal Matrix Composite Processing by the Liquid Route: Literature Contribution

NASA Astrophysics Data System (ADS)

Lacoste, Eric; Arvieu, Corinne; Mantaux, Olivier

2018-04-01

One of the technologies used to produce metal matrix composites (MMCs) is liquid route processing. One solution is to inject a liquid metal under pressure or at constant rate through a fibrous preform. This foundry technique overcomes the problem of the wettability of ceramic fibers by liquid metal. The liquid route can also be used to produce semiproducts by coating a filament with a molten metal. These processes involve physical phenomena combined with mass and heat transfer and phase change. The phase change phenomena related to solidification and also to the melting of the metal during the process notably result in modifications to the permeability of porous media, in gaps in impregnation, in the appearance of defects (porosities), and in segregation in the final product. In this article, we provide a state-of-the-art review of numerical models and simulation developed to study these physical phenomena involved in MMC processing by the liquid route.

Energy efficient engine high pressure turbine test hardware detailed design report

NASA Technical Reports Server (NTRS)

Halila, E. E.; Lenahan, D. T.; Thomas, T. T.

1982-01-01

The high pressure turbine configuration for the Energy Efficient Engine is built around a two-stage design system. Moderate aerodynamic loading for both stages is used to achieve the high level of turbine efficiency. Flowpath components are designed for 18,000 hours of life, while the static and rotating structures are designed for 36,000 hours of engine operation. Both stages of turbine blades and vanes are air-cooled incorporating advanced state of the art in cooling technology. Direct solidification (DS) alloys are used for blades and one stage of vanes, and an oxide dispersion system (ODS) alloy is used for the Stage 1 nozzle airfoils. Ceramic shrouds are used as the material composition for the Stage 1 shroud. An active clearance control (ACC) system is used to control the blade tip to shroud clearances for both stages. Fan air is used to impinge on the shroud casing support rings, thereby controlling the growth rate of the shroud. This procedure allows close clearance control while minimizing blade tip to shroud rubs.

Materials processing in space: Future technology trends

NASA Technical Reports Server (NTRS)

Barter, N. J.

1980-01-01

NASA's materials processing in space- (MPS) program involves both ground and space-based research and looks to frequent and cost effective access to the space environment for necessary progress. The first generation payloads for research are under active design and development. They will be hosted by the Space Shuttle/Spacelab on Earth orbital flights in the early 1980's. hese missions will focus on the acquisition of materials behavior research data, the potential enhancement of Earth based technology, and the implementation of space based processing for specialized, high value materials. Some materials to be studied in these payloads may provide future breakthroughs for stronger alloys, ultrapure glasses, superior electronic components, and new or better chemicals. An operational 25 kW power system is expected to be operational to support sustained, systematic space processing activity beyond shuttle capability for second generation payload systems for SPACELAB and free flyer missions to study solidification and crystal growth and to process metal/alloys, glasses/ceramics, and chemicals and biologicals.

Microstructure and crystallography of Al2O3-Y3Al5O12-ZrO2 ternary eutectic oxide grown by the micropulling down technique

NASA Astrophysics Data System (ADS)

Benamara, Omar; Cherif, Maya; Duffar, Thierry; Lebbou, Kheirreddine

2015-11-01

The directional solidification of Al2O3-YAG-ZrO2 eutectic ceramic by a micro-pulling down (μ-PD) technique is investigated. The effect of the pulling rate (0.1-1 mm min-1) on the crystallography and the microstructure is discussed. This ternary eutectic system has a Chinese script microstructure and the eutectic spacing λ depends on the pulling rate υ following the law: λ = 6.5υ-1/2 where λ is in μm and υ in μm/s as derived from the Jackson-Hunt model. With the lower pulling rates, all phases are oriented with the <100> direction parallel to the growth direction; however other orientations appear at the higher pulling rates. The Cr3+ ions R-lines emission in the sapphire phase in the ternary eutectic composite is measured to estimate the stress in the alumina phase which is also shown to depend on the pulling rate.

Space Processing Applications Rocket (SPAR) project, SPAR 9

NASA Technical Reports Server (NTRS)

Poorman, R. (Compiler)

1984-01-01

SPAR 9 (R-17) payload configuration, rocket performance, payload support, science payload instrumentation, and payload recovery are discussed. Directional solidification of magnetic composites, directional solidification of immiscible aluminum-indium alloys, and comparative alloy solidification experiments are reported.

Modelling direction solidification

NASA Technical Reports Server (NTRS)

Wilcox, W. R.

1986-01-01

The overall objective of this program is to develop an improved understanding of some phenomena of importance to directional solidification. The aim of this research is also to help predict differences in behavior between solidification on Earth and solidification in space. In this report, the validity of the Burton-Primslichter equation is explored. The influence of operating variables on grain and twin generation and propagation in single crystals of In sub (x) Ga sub (1-x) Sb is also investigated.

Optimization of Superaustenitic Stainless Steel Filler Metals for Welding Advanced Double Hull Combatant Ships

DTIC Science & Technology

2005-02-16

alloy is also given. The solidification mode of martensitic samples has been omitted and replaced with ’M’. Mo Ni +Cr Cr Ni ... alloys composed predominately of austenite. The four solidification modes present in the remaining 64 alloys , in order of increasing Cr/ Ni content, were...result in Fe- Ni -Cr-Mo alloys from the arc-melt condition. Solidification Solidification Primar- Secondar- Final microstrncture Mode

Application of Solidification Theory to Rapid Solidification Processing

DTIC Science & Technology

1983-08-01

1879 (1982). E 7] W. J. Boettinger, R. J. Schaefer, F. Biancaniello, and D. Shechtman, Met. Trans. A ., to be published. E 8] W. J. Bettinger , S. R...solidification velocity which produce a special "banded" microstructure in Ag-Cu alloys. Related lower bound to theoretical limits on solidification...partitionless rapid solidifi- cation of NiAl-Cr quasibinary eutectic alloy rather than a disordered structure incorporating Ni and Al into Cr randomly

Melt Flow Control in the Directional Solidification of Binary Alloys

NASA Technical Reports Server (NTRS)

Zabaras, Nicholas

2003-01-01

Our main project objectives are to develop computational techniques based on inverse problem theory that can be used to design directional solidification processes that lead to desired temperature gradient and growth conditions at the freezing front at various levels of gravity. It is known that control of these conditions plays a significant role in the selection of the form and scale of the obtained solidification microstructures. Emphasis is given on the control of the effects of various melt flow mechanisms on the local to the solidification front conditions. The thermal boundary conditions (furnace design) as well as the magnitude and direction of an externally applied magnetic field are the main design variables. We will highlight computational design models for sharp front solidification models and briefly discuss work in progress toward the development of design techniques for multi-phase volume-averaging based solidification models.

Nanoparticle-induced unusual melting and solidification behaviours of metals

PubMed Central

Ma, Chao; Chen, Lianyi; Cao, Chezheng; Li, Xiaochun

2017-01-01

Effective control of melting and solidification behaviours of materials is significant for numerous applications. It has been a long-standing challenge to increase the melted zone (MZ) depth while shrinking the heat-affected zone (HAZ) size during local melting and solidification of materials. In this paper, nanoparticle-induced unusual melting and solidification behaviours of metals are reported that effectively solve this long-time dilemma. By introduction of Al2O3 nanoparticles, the MZ depth of Ni is increased by 68%, while the corresponding HAZ size is decreased by 67% in laser melting at a pulse energy of 0.18 mJ. The addition of SiC nanoparticles shows similar results. The discovery of the unusual melting and solidification of materials that contain nanoparticles will not only have impacts on existing melting and solidification manufacturing processes, such as laser welding and additive manufacturing, but also on other applications such as pharmaceutical processing and energy storage. PMID:28098147

Experimental Study on the Anisotropic Stress-Strain Behavior of Polycrystalline Ni-Mn-Ga in Directional Solidification

NASA Astrophysics Data System (ADS)

Teng, Yao; Shi, Tao; Zhu, Yuping; Li, Zongbin; Deng, Tao; Bai, Guonan

2016-03-01

A polycrystalline Ni-Mn-Ga ferromagnetic shape memory alloy produced by directional solidification is the subject of this research paper. The compressive stress-strain curves of the material for different cutting angles to the solidification direction are tested. The martensite Young's modulus, macroscopic reorientation strain, and phase transition critical stress are analyzed experimentally. The results show that mechanical behaviors in the loading-unloading cycle of the material present nonlinear and anisotropic characteristics, which are all closely related to the material's orientation to the solidification direction. The martensite Young's modulus, macroscopic reorientation strain, and phase transition critical stress achieve maximum values in the solidification direction. A 50° orientation to the solidification direction is the cut-off direction of the mechanical properties, where the martensite Young's modulus and reorientation start critical stress reach minimum values. The present study is expected to provide sound guidance for practical applications.

Superior in vitro biological response and mechanical properties of an implantable nanostructured biomaterial: Nanohydroxyapatite-silicone rubber composite.

PubMed

Thein-Han, W W; Shah, J; Misra, R D K

2009-09-01

A potential approach to achieving the objective of favorably modulating the biological response of implantable biopolymers combined with good mechanical properties is to consider compounding the biopolymer with a bioactive nanocrystalline ceramic biomimetic material with high surface area. The processing of silicone rubber (SR)-nanohydroxyapatite (nHA) composite involved uniform dispersion of nHA via shear mixing and ultrasonication, followed by compounding at sub-ambient temperature, and high-pressure solidification when the final curing reaction occurs. The high-pressure solidification approach enabled the elastomer to retain the high elongation of SR even in the presence of the reinforcement material, nHA. The biological response of the nanostructured composite in terms of initial cell attachment, cell viability and proliferation was consistently greater on SR-5wt.% nHA composite surface compared to pure SR. Furthermore, in the nanocomposite, cell spreading, morphology and density were distinctly different from that of pure SR. Pre-osteoblasts grown on SR-nHA were well spread, flat, large in size with a rough cell surface, and appeared as a group. In contrast, these features were less pronounced in SR (e.g. smooth cell surface, not well spread). Interestingly, an immunofluorescence study illustrated distinct fibronectin expression level, and stronger vinculin focal adhesion contacts associated with abundant actin stress fibers in pre-osteoblasts grown on the nanocomposite compared to SR, implying enhanced cell-substrate interaction. This finding was consistent with the total protein content and SDS-PAGE analysis. The study leads us to believe that further increase in nHA content in the SR matrix beyond 5wt.% will encourage even greater cellular response. The integration of cellular and molecular biology with materials science and engineering described herein provides a direction for the development of a new generation of nanostructured materials.

Premature melt solidification during mold filling and its influence on the as-cast structure

NASA Astrophysics Data System (ADS)

Wu, M.; Ahmadein, M.; Ludwig, A.

2018-03-01

Premature melt solidification is the solidification of a melt during mold filling. In this study, a numerical model is used to analyze the influence of the pouring process on the premature solidification. The numerical model considers three phases, namely, air, melt, and equiaxed crystals. The crystals are assumed to have originated from the heterogeneous nucleation in the undercooled melt resulting from the first contact of the melt with the cold mold during pouring. The transport of the crystals by the melt flow, in accordance with the socalled "big bang" theory, is considered. The crystals are assumed globular in morphology and capable of growing according to the local constitutional undercooling. These crystals can also be remelted by mixing with the superheated melt. As the modeling results, the evolutionary trends of the number density of the crystals and the volume fraction of the solid crystals in the melt during pouring are presented. The calculated number density of the crystals and the volume fraction of the solid crystals in the melt at the end of pouring are used as the initial conditions for the subsequent solidification simulation of the evolution of the as-cast structure. A five-phase volume-average model for mixed columnar-equiaxed solidification is used for the solidification simulation. An improved agreement between the simulation and experimental results is achieved by considering the effect of premature melt solidification during mold filling. Finally, the influences of pouring parameters, namely, pouring temperature, initial mold temperature, and pouring rate, on the premature melt solidification are discussed.

Convection and Solidification with Applications to Crystal Growth

NASA Technical Reports Server (NTRS)

DeVahl Davis, Graham

1994-01-01

An outline is given of research on the directional solidification of a liquid, and of the effects of natural convection thereon. Three problems which have been studied are described. Finally, current work on solidification in microgravity conditions is discussed.

Investigation of the Relationship between Undercooling and Solidification Velocity

NASA Technical Reports Server (NTRS)

Bayuzick, Robert J.; Hofmeister, William H.

2004-01-01

This work was aimed at reconciling the differences between experimental measurements of the theoretical predictions of the solidification velocity as a function of undercooling. The theory proposed by Boettinger, Coriell and Trivedi (the BCT theory) has been one of the most widely used models for describing the nature of the solidification of undercooled metals and alloys. However, for undercoolings greater than about 5% of the absolute melting temperature, there is considerable discrepancy between theory and experiment. At these large undercoolings, experimental results exhibit a much lessened dependency of solidification velocity on undercooling than is predicted by theory. Furthermore, unpredicted plateaus in the solidification velocity as a function of undercooling are observed.

MPS Solidification Model. Volume 2: Operating guide and software documentation for the unsteady model

NASA Technical Reports Server (NTRS)

Maples, A. L.

1981-01-01

The operation of solidification Model 2 is described and documentation of the software associated with the model is provided. Model 2 calculates the macrosegregation in a rectangular ingot of a binary alloy as a result of unsteady horizontal axisymmetric bidirectional solidification. The solidification program allows interactive modification of calculation parameters as well as selection of graphical and tabular output. In batch mode, parameter values are input in card image form and output consists of printed tables of solidification functions. The operational aspects of Model 2 that differ substantially from Model 1 are described. The global flow diagrams and data structures of Model 2 are included. The primary program documentation is the code itself.

Modeling of Microstructure Evolution During Alloy Solidification

NASA Astrophysics Data System (ADS)

Zhu, Mingfang; Pan, Shiyan; Sun, Dongke

In recent years, considerable advances have been achieved in the numerical modeling of microstructure evolution during solidification. This paper presents the models based on the cellular automaton (CA) technique and lattice Boltzmann method (LBM), which can reproduce a wide variety of solidification microstructure features observed experimentally with an acceptable computational efficiency. The capabilities of the models are addressed by presenting representative examples encompassing a broad variety of issues, such as the evolution of dendritic structure and microsegregation in two and three dimensions, dendritic growth in the presence of convection, divorced eutectic solidification of spheroidal graphite irons, and gas porosity formation. The simulations offer insights into the underlying physics of microstructure formation during alloy solidification.

Monolithic All-Phosphate Solid-State Lithium-Ion Battery with Improved Interfacial Compatibility.

PubMed

Yu, Shicheng; Mertens, Andreas; Tempel, Hermann; Schierholz, Roland; Kungl, Hans; Eichel, Rüdiger-A

2018-06-22

High interfacial resistance between solid electrolyte and electrode of ceramic all-solid-state batteries is a major reason for the reduced performance of these batteries. A solid-state battery using a monolithic all-phosphate concept based on screen printed thick LiTi 2 (PO 4 ) 3 anode and Li 3 V 2 (PO 4 ) 3 cathode composite layers on a densely sintered Li 1.3 Al 0.3 Ti 1.7 (PO 4 ) 3 solid electrolyte has been realized with competitive cycling performance. The choice of materials was primarily based on the (electro-)chemical and mechanical matching of the components instead of solely focusing on high-performance of individual components. Thus, the battery utilized a phosphate backbone in combination with tailored morphology of the electrode materials to ensure good interfacial matching for a durable mechanical stability. Moreover, the operating voltage range of the active materials matches with the intrinsic electrochemical window of the electrolyte which resulted in high electrochemical stability. A highly competitive discharge capacity of 63.5 mAh g -1 at 0.39 C after 500 cycles, corresponding to 84% of the initial discharge capacity, was achieved. The analysis of interfacial charge transfer kinetics confirmed the structural and electrical properties of the electrodes and their interfaces with the electrolyte, as evidenced by the excellent cycling performance of the all-phosphate solid-state battery. These interfaces have been studied via impedance analysis with subsequent distribution of relaxation times analysis. Moreover, the prepared solid-state battery could be processed and operated in air atmosphere owing to the low oxygen sensitivity of the phosphate materials. The analysis of electrolyte/electrode interfaces after cycling demonstrates that the interfaces remained stable during cycling.

Method for preparing hydrous titanium oxide spherules and other gel forms thereof

DOEpatents

Collins, J.L.

1998-10-13

The present invention are methods for preparing hydrous titanium oxide spherules, hydrous titanium oxide gels such as gel slabs, films, capillary and electrophoresis gels, titanium monohydrogen phosphate spherules, hydrous titanium oxide spherules having suspendible particles homogeneously embedded within to form a composite sorbent, titanium monohydrogen phosphate spherules having suspendible particles of at least one different sorbent homogeneously embedded within to form a composite sorbent having a desired crystallinity, titanium oxide spherules in the form of anatase, brookite or rutile, titanium oxide spherules having suspendible particles homogeneously embedded within to form a composite, hydrous titanium oxide fiber materials, titanium oxide fiber materials, hydrous titanium oxide fiber materials having suspendible particles homogeneously embedded within to form a composite, titanium oxide fiber materials having suspendible particles homogeneously embedded within to form a composite and spherules of barium titanate. These variations of hydrous titanium oxide spherules and gel forms prepared by the gel-sphere, internal gelation process offer more useful forms of inorganic ion exchangers, catalysts, getters and ceramics. 6 figs.

Mechanical strength of ceramic scaffolds reinforced with biopolymers is comparable to that of human bone.

PubMed

Henriksen, S S; Ding, M; Juhl, M Vinther; Theilgaard, N; Overgaard, S

2011-05-01

Eight groups of calcium-phosphate scaffolds for bone implantation were prepared of which seven were reinforced with biopolymers, poly lactic acid (PLA) or hyaluronic acid in different concentrations in order to increase the mechanical strength, without significantly impairing the microarchitecture. Controls were un-reinforced calcium-phosphate scaffolds. Microarchitectural properties were quantified using micro-CT scanning. Mechanical properties were evaluated by destructive compression testing. Results showed that adding 10 or 15% PLA to the scaffold significantly increased the mechanical strength. The increase in mechanical strength was seen as a result of increased scaffold thickness and changes to plate-like structure. However, the porosity was significantly lowered as a consequence of adding 15% PLA, whereas adding 10% PLA had no significant effect on porosity. Hyaluronic acid had no significant effect on mechanical strength. The novel composite scaffold is comparable to that of human bone which may be suitable for transplantation in specific weight-bearing situations, such as long bone repair.

[Osteoconductive behaviour of beta-tricalcium phosphate ceramics in osteoporotic, metaphyseal bone defects of the distal radius].

PubMed

Hainich, J; von Rechenberg, B; Jakubietz, R G; Jakubietz, M G; Giovanoli, P; Grünert, J G

2014-02-01

Surgical treatment of osteoporotic distal radius fractures with locking plates does not completely prevent loss of reduction. Additional bone deficit stabilisation with the use of bone substitute materials is receiving increased attention. Most knowledge on the in vivo behavior of bone substitutes originates from a small number of animal models after its implantation in young, good vascularized bone. This paper investigates the osteoconductivity, resorption and biocompatibility of beta-tricalcium phosphate as a temporary bone replacement in osteoporotic type distal radius fractures. 15 bone samples taken from the augmented area of the distal radius of elderly people during metal removal were examined. The material was found to be osteoconductive, good degradable, and biocompatible. Degrading process and remodelling to woven bone seem to require more time than in available comparative bioassays. The material is suitable for temporary replacement of lost, distal radius bone from the histological point of view. © Georg Thieme Verlag KG Stuttgart · New York.

Crystallization, fluoridation and some properties of apatite thin films prepared through rf-sputtering from CaO-P2O5 glasses.

PubMed

Yamashita, K; Matsuda, M; Arashi, T; Umegaki, T

1998-07-01

Using calcium phosphate glass targets with the CaO/P2O5 molar ratios of 1.50-0.50, much lower than the stoichiometric value of 3.3 for hydroxyapatite, thin films of stoichiometric hydroxy-, nonstoichiometric oxyhydroxy- and Ca-deficient oxyhydroxy-apatites were prepared on alumina ceramic substrates by rf-sputtering followed by post-annealing. Based on the present results, a phase diagram for CaO-P2O5 at low temperatures in the ambience of air was depicted for thin films. The ambient H2O vapor had an influence on the phase diagram: Tricalcium phosphate was changed to apatite in the presence of H2O vapor. Dense fluorohydroxyapatite thin films were prepared by fluoridation of those apatite thin films at a low temperature such as 200 degrees C. In the present report, some functional properties of thin films thus prepared were also shown.

Method for preparing hydrous titanium oxide spherules and other gel forms thereof

DOEpatents

Collins, Jack L.

1998-01-01

The present invention are methods for preparing hydrous titanium oxide spherules, hydrous titanium oxide gels such as gel slabs, films, capillary and electrophoresis gels, titanium monohydrogen phosphate spherules, hydrous titanium oxide spherules having suspendible particles homogeneously embedded within to form a composite sorbent, titanium monohydrogen phosphate spherules having suspendible particles of at least one different sorbent homogeneously embedded within to form a composite sorbent having a desired crystallinity, titanium oxide spherules in the form of anatase, brookite or rutile, titanium oxide spherules having suspendible particles homogeneously embedded within to form a composite, hydrous titanium oxide fiber materials, titanium oxide fiber materials, hydrous titanium oxide fiber materials having suspendible particles homogeneously embedded within to form a composite, titanium oxide fiber materials having suspendible particles homogeneously embedded within to form a composite and spherules of barium titanate. These variations of hydrous titanium oxide spherules and gel forms prepared by the gel-sphere, internal gelation process offer more useful forms of inorganic ion exchangers, catalysts, getters and ceramics.

Effect of solidification rate on microstructure evolution in dual phase microalloyed steel

PubMed Central

Kostryzhev, A. G.; Slater, C. D.; Marenych, O. O.; Davis, C. L.

2016-01-01

In steels the dependence of ambient temperature microstructure and mechanical properties on solidification rate is not well reported. In this work we investigate the microstructure and hardness evolution for a low C low Mn NbTi-microalloyed steel solidified in the cooling rate range of 1–50 Cs−1. The maximum strength was obtained at the intermediate solidification rate of 30 Cs−1. This result has been correlated to the microstructure variation with solidification rate. PMID:27759109

Al and Mg Alloys for Aerospace Applications Using Rapid Solidification and Power Metallurgy Processing.

DTIC Science & Technology

1981-10-07

primary solidification phase in the alloy in this condition was identified by CBED as Mg 2 Si , which formed dendrites within the matrix. Each... solidification below the extended c-liquidus. Evolution of Microstructure in Melt-spun Mg- Si Alloys -, The microstructurcs observed in the alloys can...solidificaion pr(es .. in the cellular (dendritic) regime. Solidification of the 5.0 wt.% Si alloy occurs in the coupled eutectic region, and the 8.0 wt.% Si

Rapid solidification of levitation melted Ni-Sn alloy droplets with high undercooling

NASA Technical Reports Server (NTRS)

Shiohara, Yuh; Flemings, Merton C.; Wu, Yanzhong; Piccone, Thomas J.

1985-01-01

Experimental results obtained by high-speed optical temperature sensing for the rapid solidification of highly undercooled, levitation-melted Ni-Sn alloy droplets are presented. These data suggest a solidification model proceeding according to overlapping steps: (1) dendritic growth within the bulk undercooled melt, (2) continued recalescence as supersaturation of the interdendritic liquid dissipates, (3) fine-scale remelting within the dendrites, (4) ripening of the fine structure, and (5) solidification of remaining liquid at the end of recalescence.

Fundamentals of rapid solidification processing

NASA Technical Reports Server (NTRS)

Flemings, Merton C.; Shiohara, Yuh

1985-01-01

An attempt is made to illustrate the continuous change that occurs in the solidification behavior of undercooled melts, as cooling rates increase from 0.0001 K/sec to about 1000 K/sec. At the higher cooling rates, more significant changes occur as the dendrite tip temperature begins to drop from the equilibrium liquidus. Discontinuous solidification behavior changes will occur if absolute stability is reached, or a metastable phase forms, or solidification proceeds to a glass rather than to a crystalline solid, or if there is significant undercooling prior to nucleation.

Characteristics of solidified products containing radioactive molten salt waste.

PubMed

Park, Hwan-Seo; Kim, In-Tae; Cho, Yong-Zun; Eun, Hee-Chul; Kim, Joon-Hyung

2007-11-01

The molten salt waste from a pyroprocess to recover uranium and transuranic elements is one of the problematic radioactive wastes to be solidified into a durable wasteform for its final disposal. By using a novel method, named as the GRSS (gel-route stabilization/solidification) method, a molten salt waste was treated to produce a unique wasteform. A borosilicate glass as a chemical binder dissolves the silicate compounds in the gel products to produce one amorphous phase while most of the phosphates are encapsulated by the vitrified phase. Also, Cs in the gel product is preferentially situated in the silicate phase, and it is vitrified into a glassy phase after a heat treatment. The Sr-containing phase is mainly phosphate compounds and encapsulated by the glassy phase. These phenomena could be identified by the static and dynamic leaching test that revealed a high leach resistance of radionuclides. The leach rates were about 10(-3) - 10(-2) g/m2 x day for Cs and 10(-4) - 10(-3) g/m2 x day for Sr, and the leached fractions of them were predicted to be 0.89% and 0.39% at 900 days, respectively. This paper describes the characteristics of a unique wasteform containing a molten salt waste and provides important information on a newly developed immobilization technology for salt wastes, the GRSS method.

Phase Equilibria Diagrams Database

National Institute of Standards and Technology Data Gateway

SRD 31 NIST/ACerS Phase Equilibria Diagrams Database (PC database for purchase)   The Phase Equilibria Diagrams Database contains commentaries and more than 21,000 diagrams for non-organic systems, including those published in all 21 hard-copy volumes produced as part of the ACerS-NIST Phase Equilibria Diagrams Program (formerly titled Phase Diagrams for Ceramists): Volumes I through XIV (blue books); Annuals 91, 92, 93; High Tc Superconductors I & II; Zirconium & Zirconia Systems; and Electronic Ceramics I. Materials covered include oxides as well as non-oxide systems such as chalcogenides and pnictides, phosphates, salt systems, and mixed systems of these classes.

A comparative study of the proliferation and osteogenic differentiation of human periodontal ligament cells cultured on β-TCP ceramics and demineralized bone matrix with or without osteogenic inducers in vitro.

PubMed

An, Shaofeng; Gao, Yan; Huang, Xiangya; Ling, Junqi; Liu, Zhaohui; Xiao, Yin

2015-05-01

The repair of bone defects that result from periodontal diseases remains a clinical challenge for periodontal therapy. β-tricalcium phosphate (β-TCP) ceramics are biodegradable inorganic bone substitutes with inorganic components that are similar to those of bone. Demineralized bone matrix (DBM) is an acid-extracted organic matrix derived from bone sources that consists of the collagen and matrix proteins of bone. A few studies have documented the effects of DBM on the proliferation and osteogenic differentiation of human periodontal ligament cells (hPDLCs). The aim of the present study was to investigate the effects of inorganic and organic elements of bone on the proliferation and osteogenic differentiation of hPDLCs using three-dimensional porous β-TCP ceramics and DBM with or without osteogenic inducers. Primary hPDLCs were isolated from human periodontal ligaments. The proliferation of the hPDLCs on the scaffolds in the growth culture medium was examined using a Cell-Counting kit-8 (CCK-8) and scanning electron microscopy (SEM). Alkaline phosphatase (ALP) activity and the osteogenic differentiation of the hPDLCs cultured on the β-TCP ceramics and DBM were examined in both the growth culture medium and osteogenic culture medium. Specific osteogenic differentiation markers were examined using reverse transcription-quantitative polymerase chain reaction (RT-qPCR). SEM images revealed that the cells on the β-TCP were spindle-shaped and much more spread out compared with the cells on the DBM surfaces. There were no significant differences observed in cell proliferation between the β-TCP ceramics and the DBM scaffolds. Compared with the cells that were cultured on β-TCP ceramics, the ALP activity, as well as the Runx2 and osteocalcin (OCN) mRNA levels in the hPDLCs cultured on DBM were significantly enhanced both in the growth culture medium and the osteogenic culture medium. The organic elements of bone may exhibit greater osteogenic differentiation effects on hPDLCs than the inorganic elements.

Materials Science Laboratory - Columnar-to-Equiaxed Transition in Solidification Processing and Microstructure Formation in Casting of Technical Alloys under Diffusive and Magnetically Controlled Convective Conditions

NASA Technical Reports Server (NTRS)

Gandin, Charles-Andre; Ratke, Lorenz

2008-01-01

The Materials Science Laboratory - Columnar-to-Equiaxed Transition in Solidification Processing and Microstructure Formation in Casting of Technical Alloys under Diffusive and Magnetically Controlled Convective Conditions (MSL-CETSOL and MICAST) are two investigations which supports research into metallurgical solidification, semiconductor crystal growth (Bridgman and zone melting), and measurement of thermo-physical properties of materials. This is a cooperative investigation with the European Space Agency (ESA) and National Aeronautics and Space Administration (NASA) for accommodation and operation aboard the International Space Station (ISS). Research Summary: Materials Science Laboratory - Columnar-to-Equiaxed Transition in Solidification Processing (CETSOL) and Microstructure Formation in Casting of Technical Alloys under Diffusive and Magnetically Controlled Convective Conditions (MICAST) are two complementary investigations which will examine different growth patterns and evolution of microstructures during crystallization of metallic alloys in microgravity. The aim of these experiments is to deepen the quantitative understanding of the physical principles that govern solidification processes in cast alloys by directional solidification.

Stability of the bond between two resin cements and an yttria-stabilized zirconia ceramic after six months of aging in water.

PubMed

da Silva, Eduardo M; Miragaya, Luciana; Sabrosa, Carlos Eduardo; Maia, Lucianne C

2014-09-01

The behavior of the luting cement and the cementation protocol are essential in the clinical success of ceramic restorations. The purpose of this study was to evaluate the bond stability of 2 resin cements and a yttria-stabilized tetragonal polycrystalline zirconia (Y-TZP) ceramic submitted to 2 surface treatments. Sixty plates of a Y-TZP ceramic were assigned to 3 groups according to the surface treatments: control, as sintered surface; methacryloxydecyl dihydrogen phosphate (MDP), coated with an MDP-based primer, and tribochemical silica-coating (TSC), coated with tribochemical silica. The plates of each group were further divided into 2 subgroups according to the resin cement as follows: RelyX adhesive resin cement (conventional) and RelyX Unicem (self-adhesive). Cylinders of resin cements (∅=0.75 mm × 0.5 mm in height) were built up on the ceramic surfaces, and the plates stored in distilled water at 37°C for either 24 hours or 6 months before being submitted to a microshear bond strength test. The data were submitted to 3-way ANOVA and the Tukey honestly significant difference test (α=.05). Three-way ANOVA showed statistical significance for the 3 independent factors: resin cement, surface treatment, and period of water immersion (P<.001). Unicem presented the highest microshear bond strength after 24 hours (MDP, 37.4 ±2.3 and TSC, 36.2 ±2.1 MPa). Except for RelyX adhesive resin cement applied on ceramic surfaces treated with TSC, the microshear bond strength of all the other groups decreased after 6 months of aging in water. The microshear bond strength decreased most in the control groups (-81.5% for ARC and -93.1% for Unicem). In the group treated with TSC, the microshear bond strength for Unicem decreased by 54.8% and in that treated with MDP-based primer by -42.5%. In the group treated with MDP-based primer, the microshear bond strength for RelyX ARC decreased by -52.8%. Irrespective of surface treatments, self-adhesive resin cement was not able to maintain the bond to Y-TZP ceramic after 6 months of aging in water. Copyright © 2014 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

Technology Performance Review: Selecting And Using Solidification/Stabilization Treatment For Site Remediation

EPA Science Inventory

Solidification/Stabilization (S/S) is a widely used treatment technology to prevent migration and exposure of contaminants from a contaminated media (i.e., soil, sludge and sediment). Solidification refers to a process that binds a contaminated media with a reagent changing its ...

Durability of resin cement bond to aluminium oxide and zirconia ceramics after air abrasion and laser treatment.

PubMed

Foxton, Richard M; Cavalcanti, Andrea N; Nakajima, Masatoshi; Pilecki, Peter; Sherriff, Martyn; Melo, Luciana; Watson, Timothy F

2011-02-01

The erbium laser has been introduced for cutting enamel and dentin and may have an application in the surface modification of high-strength aluminum oxide and zirconia ceramics. The aim of this study was to evaluate the durability of the bond of conventional dual-cured resin cements to Procera Al(2)O(3) and zirconium oxide ceramics after surface treatment with air abrasion and erbium laser. One hundred twenty Al(2)O(3) and 120 zirconia specimens measuring 3 × 3 × 0.7 mm(3) were divided equally into three groups, and their surfaces treated as follows: either untreated (controls), air abraded with Al(2)O(3) particles, or erbium-laser-treated at a power setting of 200 mJ. The surface of each specimen was then primed and bonded with one of two dual-cured resin cements (either SCP-100 Ceramic Primer and NAC-100 or Monobond S and Variolink II) using a 1-mm thick Tygon tube mold with a 0.75-mm internal bore diameter. After 24 hours and 6 months of water storage at 37°C, a microshear bond strength test was performed at a crosshead speed of 1 mm/min. Surface morphology was examined using a confocal microscope, and failure modes were observed using an optical microscope. The data were analyzed using the Kaplan-Meier nonparametric survival analysis. In the case of zirconia, air abrasion and Erbium:yttrium-aluminum-garnet (Er:YAG) laser treatment of the ceramic surface resulted in a significant reduction in the bond strengths of both resin cements after 6 months water storage; however, when the zirconia surface was left untreated, the SCP-100/NAC-100 group did not significantly reduce in bond strength. In the case of alumina, no treatment, air abrasion and Er:YAG laser treatment of the surface led to no significant reduction in the bond strengths of the three SCP-100/NAC-100 groups after 6 months water storage, whereas all three Monobond S/Variolink II groups showed a significant reduction. Er:YAG laser treatment of the zirconia surface did not result in a durable resin cement/ceramic bond; however, a durable bond between a conventional dual-cured resin cement and Procera All Ceram and Procera All Zirkon was formed using a ceramic primer containing the phosphate monomer, MDP, without any additional surface treatment. © 2011 by The American College of Prosthodontists.

Influence of microstructure and AlPO4 secondary-phase on the ionic conductivity of Li1.3Al0.3Ti1.7(PO4)3 solid-state electrolyte

NASA Astrophysics Data System (ADS)

Yu, Shicheng; Mertens, Andreas; Gao, Xin; Gunduz, Deniz Cihan; Schierholz, Roland; Benning, Svenja; Hausen, Florian; Mertens, Josef; Kungl, Hans; Tempel, Hermann; Eichel, Rüdiger-A.

2016-09-01

A ceramic solid-state electrolyte of lithium aluminum titanium phosphate with the composition of Li1.3Al0.3Ti1.7(PO4)3 (LATP) was synthesized by a sol-gel method using a pre-dissolved Ti-source. The annealed LATP powders were subsequently processed in a binder-free dry forming method and sintered under air for the pellet preparation. Phase purity, density, microstructure as well as ionic conductivity of the specimen were characterized. The highest density (2.77gṡcm-3) with an ionic conductivity of 1.88×10-4 Sṡcm-1 (at 30∘C) was reached at a sintering temperature of 1100∘C. Conductivity of LATP ceramic electrolyte is believed to be significantly affected by both, the AlPO4 secondary phase content and the ceramic electrolyte microstructure. It has been found that with increasing sintering temperature, the secondary-phase content of AlPO4 increased. For sintering temperatures above 1000∘C, the secondary phase has only a minor impact, and the ionic conductivity is predominantly determined by the microstructure of the pellet, i.e. the correlation between density, porosity and particle size. In that respect, it has been demonstrated, that the conductivity increases with increasing particle size in this temperature range and density.

Electrochemical Cell for Obtaining Oxygen from Carbon Dioxide Atmospheres

NASA Technical Reports Server (NTRS)

Hooker, Matthew; Rast, H. Edward; Rogers, Darren K.; Borja, Luis; Clark, Kevin; Fleming, Kimberly; Mcgurren, Michael; Oldaker, Tom; Sweet, Nanette

1989-01-01

To support human life on the Martian surface, an electrochemical device will be required to obtain oxygen from the carbon dioxide rich atmosphere. The electrolyte employed in such a device must be constructed from extremely thin, dense membranes to efficiently acquire the oxygen necessary to support life. A forming process used industrially in the production of multilayer capacitors and electronic substrates was adapted to form the thin membranes required. The process, known as the tape casting, involves the suspension consisting of solvents and binders. The suspension is passed under a blade, resulting in the production of ceramic membranes between 0.1 and 0.5 mm thick. Once fired, the stabilized zirconia membranes were assembled into the cell design by employing a zirconium phosphate solution as the sealing agent. The resulting ceramic-to-ceramic seals were found to be structurally sound and gas-tight. Furthermore, by using a zirconia-based solution to assemble the cell, the problem of a thermal expansion mismatch was alleviated. By adopting an industrial forming process to produce thin membranes, an electrochemical cell for obtaining oxygen from carbon dioxide was produced. The proposed cell design is unique in that it does not require a complicated manifold system for separating the various gases present in this process, nor does it require a series of complex electrical connections. Thus, the device can reliably obtain the vital oxygen supply from the toxic carbon dioxide atmosphere.

Current progress in inorganic artificial biomaterials.

PubMed

Li, Zhixia; Kawashita, Masakazu

2011-09-01

In this review, recent advances in bioceramics, metallic biomaterials, and their composites are discussed in terms of their material properties and new medical applications. Porous calcium phosphate ceramics have attracted a lot attention as scaffolds for tissue-engineering purposes since the porous structure allows bone ingrowth. The addition of biodegradable polymers like chitosan, gelatin, and collagen have modified the degradability of the ceramics and their mechanical properties. Titanium (Ti) alloys are being developed for the fabrication of medical devices for the replacement of hard tissue such as artificial hip joints, bone plates, and dental implants because they are very reliable from the viewpoint of mechanical performance. Physical treatment such as grooving or setting a spatial gap on the surface of materials is applicable to improve the apatite formation on the Ti alloys. Blood-compatible polymers such as poly(ethylene glycol) have been successfully fixed on the surface of Ti via chemical bonding by an electrodeposition method. New functions have been explored in Ni-free, Co-Cr-Mo alloys and Mg alloys. In addition, yttrium-containing or phosphorus-containing glass microspheres (20-30 μm in diameter) and ferrimagnetic ceramic particles have exhibited great potential to realize minimally invasive treatment of cancer without surgical operation via in situ radiotherapy or hyperthermia of cancer, but it is still a major challenge to clarify the biological reaction between the artificial implants and living body before their application.

Effect of the temperature-rate parameters of directional solidification on the structure formation in high-temperature materials

NASA Astrophysics Data System (ADS)

Svetlov, I. L.; Neiman, A. V.

2017-03-01

The effect of the temperature gradient and the crystal growth rate on the structure formation in nickel and niobium superalloys is studied under the conditions of the flat, cellular, dendritic, or dendritic-cellular configuration of a solidification front during directional solidification.

Analysis and calculation of macrosegregation in a casting ingot. MPS solidification model. Volume 2: Software documentation

NASA Technical Reports Server (NTRS)

Maples, A. L.

1980-01-01

The software developed for the solidification model is presented. A link between the calculations and the FORTRAN code is provided, primarily in the form of global flow diagrams and data structures. A complete listing of the solidification code is given.

SOLIDIFICATION/STABILIZATION FOR REMEDIATON OF WOOD PRESERVING SITES: TREATMENT FOR DIOXINS, PCP, CREOSOTE, AND METALS

EPA Science Inventory

This article discusses the use of solidification/stabilization (S/S) to treat soils contaminated with organic and inorganic chemicals at wood preserving sites. Solidification is defined for this article as making a material into a free standing solid. Stabilization is defined as ...

Numerical simulation of freckle formation in directional solidification of binary alloys

NASA Technical Reports Server (NTRS)

Felicelli, Sergio D.; Heinrich, Juan C.; Poirier, David R.

1992-01-01

A mathematical model of solidification is presented which simulates the formation of segregation models known as 'freckles' during directional solidification of binary alloys. The growth of the two-phase or dendritic zone is calculated by solving the coupled equations of momentum, energy, and solute transport, as well as maintaining the thermodynamic constraints dictated by the phase diagram of the alloy. Calculations for lead-tin alloys show that the thermosolutal convection in the dendritic zone during solidification can produce heavily localized inhomogeneities in the composition of the final alloy.

Microsegregation during directional solidification

NASA Technical Reports Server (NTRS)

Coriell, S. R.; Mcfadden, G. B.

1984-01-01

During the directional solidification of alloys, solute inhomogeneities transverse to the growth direction arise due to morphological instabilities (leading to cellular or dendritic growth) and/or due to convection in the melt. In the absence of convection, the conditions for the onset of morphological instability are given by the linear stability analysis of Mullins and Sekerka. For ordinary solidification rates, the predictions of linear stability analysis are similar to the constitutional supercooling criterion. However, at very rapid solidification rates, linear stability analysis predicts a vast increase in stabilization in comparison to constitutional supercooling.

Evolution of solidification texture during additive manufacturing.

PubMed

Wei, H L; Mazumder, J; DebRoy, T

2015-11-10

Striking differences in the solidification textures of a nickel based alloy owing to changes in laser scanning pattern during additive manufacturing are examined based on theory and experimental data. Understanding and controlling texture are important because it affects mechanical and chemical properties. Solidification texture depends on the local heat flow directions and competitive grain growth in one of the six <100> preferred growth directions in face centered cubic alloys. Therefore, the heat flow directions are examined for various laser beam scanning patterns based on numerical modeling of heat transfer and fluid flow in three dimensions. Here we show that numerical modeling can not only provide a deeper understanding of the solidification growth patterns during the additive manufacturing, it also serves as a basis for customizing solidification textures which are important for properties and performance of components.

In Situ X-Ray Observations of Dendritic Fragmentation During Directional Solidification of a Sn-Bi Alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gibbs, John W.; Tourret, Damien; Gibbs, Paul J.

2015-09-25

Dendrite fragmentation is an important phenomenon in microstructural development during solidification. For instance, it plays a key role in initiating the columnar-to-equiaxed transition (CET). Here, we use x-ray radiography to study dendrite fragmentation rate in a Sn-39.5 wt.% Bi alloy during directional solidification. Experiments were performed in which solidification was parallel and anti-parallel to gravity, leading to significantly different fragmentation rates. We quantify the distribution of fragmentation rate as a function of distance from the solidification front, time in the mushy zone, and volume fraction of solid. While the observed fragmentation rate can be high, there is no evidence ofmore » a CET, illustrating that it requires more than just fragmentation to occur.« less

Scaling Analysis of Alloy Solidification and Fluid Flow in a Rectangular Cavity

NASA Astrophysics Data System (ADS)

Plotkowski, A.; Fezi, K.; Krane, M. J. M.

A scaling analysis was performed to predict trends in alloy solidification in a side-cooled rectangular cavity. The governing equations for energy and momentum were scaled in order to determine the dependence of various aspects of solidification on the process parameters for a uniform initial temperature and an isothermal boundary condition. This work improved on previous analyses by adding considerations for the cooling bulk fluid flow. The analysis predicted the time required to extinguish the superheat, the maximum local solidification time, and the total solidification time. The results were compared to a numerical simulation for a Al-4.5 wt.% Cu alloy with various initial and boundary conditions. Good agreement was found between the simulation results and the trends predicted by the scaling analysis.

Efficient estimation of diffusion during dendritic solidification

NASA Technical Reports Server (NTRS)

Yeum, K. S.; Poirier, D. R.; Laxmanan, V.

1989-01-01

A very efficient finite difference method has been developed to estimate the solute redistribution during solidification with diffusion in the solid. This method is validated by comparing the computed results with the results of an analytical solution derived by Kobayashi (1988) for the assumptions of a constant diffusion coefficient, a constant equilibrium partition ratio, and a parabolic rate of the advancement of the solid/liquid interface. The flexibility of the method is demonstrated by applying it to the dendritic solidification of a Pb-15 wt pct Sn alloy, for which the equilibrium partition ratio and diffusion coefficient vary substantially during solidification. The fraction eutectic at the end of solidification is also obtained by estimating the fraction solid, in greater resolution, where the concentration of solute in the interdendritic liquid reaches the eutectic composition of the alloy.

The growth of metastable peritectic compounds

NASA Technical Reports Server (NTRS)

Larson, D. J., Jr.

1984-01-01

The influence of gravitationally driven convection on the directional solidification of peritectic alloys was evaluated. The Pb-Bi peritectic was studied as a model solidification system. Analyses of directionally solidified Pb-Bi peritectic samples indicate that appreciable macrosegregation occurs due to thermosolutal convection and/or Soret diffusion. The macrosegregation results in sequantial change of phase and morphology as solidification progresses down the length of the sample. Banding was eliminated when furnace conditions were selected which resulted in a planar solidification interface. The directional solidification that occurs in the vicinity of the Pb-Bi peritectic isothermal was found to be isocompositional and to consist solely of the equilibrium terminal solid solution and peritectic phases on an extremely fine scale. Evidence was found to support the peritectic supercooling mechanism, but not the proposed peritectic superheat mechanism.

In Situ X-Ray Observations of Dendritic Fragmentation During Directional Solidification of a Sn-Bi Alloy

DOE PAGES

Gibbs, John W.; Tourret, Damien; Gibbs, Paul J.; ...

2015-09-25

Dendrite fragmentation is an important phenomenon in microstructural development during solidification. For instance, it plays a key role in initiating the columnar-to-equiaxed transition (CET). In this paper, we use x-ray radiography to study dendrite fragmentation rate in a Sn-39.5 wt.% Bi alloy during directional solidification. Experiments were performed in which solidification was parallel and anti-parallel to gravity, leading to significantly different fragmentation rates. We quantify the distribution of fragmentation rate as a function of distance from the solidification front, time in the mushy zone, and volume fraction of solid. Finally, while the observed fragmentation rate can be high, there ismore » no evidence of a CET, illustrating that it requires more than just fragmentation to occur.« less

Multiscale X-ray and Proton Imaging of Bismuth-Tin Solidification

NASA Astrophysics Data System (ADS)

Gibbs, P. J.; Imhoff, S. D.; Morris, C. L.; Merrill, F. E.; Wilde, C. H.; Nedrow, P.; Mariam, F. G.; Fezzaa, K.; Lee, W.-K.; Clarke, A. J.

2014-08-01

The formation of structural patterns during metallic solidification is complex and multiscale in nature, ranging from the nanometer scale, where solid-liquid interface properties are important, to the macroscale, where casting mold filling and intended heat transfer are crucial. X-ray and proton imaging can directly interrogate structure, solute, and fluid flow development in metals from the microscale to the macroscale. X-rays permit high spatio-temporal resolution imaging of microscopic solidification dynamics in thin metal sections. Similarly, high-energy protons permit imaging of mesoscopic and macroscopic solidification dynamics in large sample volumes. In this article, we highlight multiscale x-ray and proton imaging of bismuth-tin alloy solidification to illustrate dynamic measurement of crystal growth rates and solute segregation profiles that can be that can be acquired using these techniques.

Modeling of Rapid Solidification with Undercooling Effect During Droplet Flattening on a Substrate in Coating Formation

NASA Astrophysics Data System (ADS)

Shukla, Rajesh Kumar; Patel, Virendra; Kumar, Arvind

2018-02-01

The coating deposit on the substrate in thermal spray coating process develops by solidification of individual molten particle which impacts, flattens and solidifies on the surface of the substrate. Droplet flattening and solidification typically involves rapid cooling. In this paper, a model for non-equilibrium rapid solidification of a molten droplet spreading onto a substrate is presented. Transient flow during droplet impact and its subsequent spreading is considered using the volume of fluid surface tracking method which was fully coupled with the rapid solidification model. The rapid solidification model includes undercooling, nucleation, interface tracking, non-equilibrium solidification kinetics and combined heat transfer and fluid flow as required to treat a non-stagnant splat formed from droplet flattening. The model is validated with the literature results on stagnant splats. Subsequently, using the model the characteristics of the rapidly solidifying interface for non-stagnant splat, such as interface velocity and interface temperature, are described and the effect of undercooling and interfacial heat transfer coefficient are highlighted. In contrast to the stagnant splat, the non-stagnant splat considered in this study displays interesting features in the rapidly solidifying interface. These are attributed to droplet thinning and droplet recoiling that occur during the droplet spreading process.

Utilization of coal fly ash in solidification of liquid radioactive waste from research reactor.

PubMed

Osmanlioglu, Ahmet Erdal

2014-05-01

In this study, the potential utilization of fly ash was investigated as an additive in solidification process of radioactive waste sludge from research reactor. Coal formations include various percentages of natural radioactive elements; therefore, coal fly ash includes various levels of radioactivity. For this reason, fly ashes have to be evaluated for potential environmental implications in case of further usage in any construction material. But for use in solidification of radioactive sludge, the radiological effects of fly ash are in the range of radioactive waste management limits. The results show that fly ash has a strong fixing capacity for radioactive isotopes. Specimens with addition of 5-15% fly ash to concrete was observed to be sufficient to achieve the target compressive strength of 20 MPa required for near-surface disposal. An optimum mixture comprising 15% fly ash, 35% cement, and 50% radioactive waste sludge could provide the solidification required for long-term storage and disposal. The codisposal of radioactive fly ash with radioactive sludge by solidification decreases the usage of cement in solidification process. By this method, radioactive fly ash can become a valuable additive instead of industrial waste. This study supports the utilization of fly ash in industry and the solidification of radioactive waste in the nuclear industry.

Solidification characteristics and segregation behavior of a P-containing Ni-Fe-Cr-based alloy

NASA Astrophysics Data System (ADS)

Wang, Changshuai; Su, Haijun; Guo, YongAn; Guo, Jianting; Zhou, Lanzhang

2017-09-01

Solidification characteristics and segregation behavior of a P-containing Ni-Fe-Cr-based alloy, considered as boiler and turbine materials in 700 °C advanced ultra-supercritical coal-fired power plants, have been investigated by differential thermal analysis and directional solidification quenching technique. Results reveal that P decreases the solidus temperature, but only has negligible influence on liquidus temperature. After P was added, the solidification sequence has no apparent change, but the width of the mushy zone increases and dendritic structures become coarser. Moreover, P increases the amount and changes the morphology of MC carbide. Energy-dispersive spectroscopy analysis reveals that P has obvious influence on the segregation behavior of the constitute elements with equilibrium partition coefficients (ki) far away from unity, whereas has negligible effect on the constituent elements with ki close to unity and has more influence on the final stage of solidification than at early stage. The distribution profiles reveal that P atoms pile up ahead of the solid/liquid (S/L) interface and strongly segregate to the interdendritic liquid region. The influence of P on solidification characteristics and segregation behavior of Ni-Fe-Cr-based alloy could be attributed to the accumulation of P ahead of the S/L interface during solidification.

Timing of mantle overturn during magma ocean solidification

NASA Astrophysics Data System (ADS)

Boukaré, C.-E.; Parmentier, E. M.; Parman, S. W.

2018-06-01

Solidification of magma oceans (MOs) formed early in the evolution of planetary bodies sets the initial condition for their evolution on much longer time scales. Ideal fractional crystallization would generate an unstable chemical stratification that subsequently overturns to form a stably stratified mantle. The simplest model of overturn assumes that cumulates remain immobile until the end of MO solidification. However, overturning of cumulates and thermal convection during solidification may act to reduce this stratification and introduce chemical heterogeneity on scales smaller than the MO thickness. We explore overturning of cumulates before the end of MO crystallization and the possible consequences for mantle structure and composition. In this model, increasingly dense iron-rich layers, crystallized from the overlying residual liquid MO, are deposited on a thickening cumulate layer. Overturn during solidification occurs if the dimensionless parameter, Rc, measuring the ratio of the MO time of crystallization τMO to the timescale associated with compositional overturn τov = μ / ΔρgH exceeds a threshold value. If overturn did not occur until after solidification, this implies that the viscosity of the solidified mantle must have been sufficiently high (possibly requiring efficient melt extraction from the cumulate) for a given rate of solidification. For the lunar MO, possible implications for the generation of the Mg-suites and mare basalt are suggested.

The effects of solidification on sill propagation dynamics and morphology

NASA Astrophysics Data System (ADS)

Chanceaux, L.; Menand, T.

2016-05-01

Sills are an integral part of the formation and development of larger plutons and magma reservoirs. Thus sills are essential for both the transport and the storage of magma in the Earth's crust. However, although cooling and solidification are central to magmatism, their effects on sills have been so far poorly studied. Here, the effects of solidification on sill propagation dynamics and morphology are studied by means of analogue laboratory experiments. Hot fluid vegetable oil (magma analogue), that solidifies during its propagation, is injected as a sill in a colder layered gelatine solid (elastic host rock analogue). The injection flux and temperature are maintained constant during an experiment and systematically varied between each experiment, in order to vary and quantify the amount of solidification between each experiments. The oil is injected directly at the interface between the two gelatine layers. When solidification effects are small (high injection temperatures and fluxes), the propagation is continuous and the sill has a regular and smooth surface. Inversely, when solidification effects are important (low injection temperatures and fluxes), sill propagation is discontinuous and occurs by steps of surface-area creation interspersed with periods of momentary arrest. The morphology of these sills displays folds, ropy structures on their surface, and lobes with imprints of the leading fronts that correspond to each step of area creation. These experiments show that for a given, constant injected volume, as solidification effects increase, the area of the sills decreases, their thickness increases, and the number of propagation steps increases. These results have various geological and geophysical implications. The morphology of sills, such as lobate structures (interpretation of 3D seismic studies in sedimentary basin) and ropy flow structures (field observations) can be related to solidification during emplacement. Moreover, a non-continuous morphology as observed in the field does not necessarily involve multiple injections, but could instead reflect a continuous, yet complex morphology induced by solidification effects during emplacement. Also, a discontinuous sill propagation induced by solidification effects should be associated with bursts of seismic activity. Finally, our study shows that once a sill has initiated, the dimensionless flux influences the sill thermal state, and in turn its propagation, and final extent and thickness. In restricting the lateral extent of sills, magma cooling and solidification are likely to impact directly the size of plutons constructed by amalgamated sills.

Characteristics of hydroxyapatite coated titanium porous coatings on Ti-6Al-4V substrates by plasma sprayed method.

PubMed

Yang, C Y; Chen, C R; Chang, E; Lee, T M

2007-08-01

A porous metal coating applied to solid substrate implants has been shown, in vivo, to anchor implants by bone ingrowth. Calcium phosphate ceramics, in particular hydroxyapatite [Ca(10)(PO(4))(6)(OH)(2), HA], are bioactive ceramics, which are known to be biocompatible and osteoconductive, and these ceramics deposited on to porous-coated devices may enhance bone ingrowth and implant fixation. In this study, bi-feedstock of the titanium powder and composite (Na(2)CO(3)/HA) powder were simultaneously deposited on a Ti-6Al-4V substrate by a plasma sprayed method. At high temperature of plasma torch, the solid state of Na(2)CO(3) would decompose to release CO(2) gas and then eject the molten Ti powder to induce the interconnected pores in the coatings. After cleaning and soaking in deionized water, the residual Na(2)CO(3) in the coating would dissolve to form the open pores, and the HA would exist at the surface of pores in the inner coatings. By varying the particle size of the composite powder, the porosity of porous coating could be varied from 25.0 to 34.0%, and the average pore size of the porous coating could be varied to range between 158.5 and 202.0 microm. Using a standard adhesive test (ASTM C-633), the bonding strength of the coating is between 27.3 and 38.2 MPa. By SEM, the HA was observed at the surface of inner pore in the porous coating. These results suggest that the method exhibits the potential to manufacture the bioactive ceramics on to porous-coated specimen to achieve bone ingrowth fixation for biomedical applications.

Optimization of an enhanced ceramic micro-filter for concentrating E.coli in water

NASA Astrophysics Data System (ADS)

Zhang, Yushan; Guo, Tianyi; Xu, Changqing; Hong, Lingcheng

2017-02-01

Recently lower limit of detection (LOD) is necessary for rapid bacteria detection and analysis applications in clinical practices and daily life. A critical pre-conditioning step for these applications is bacterial concentration, especially for low level of pathogens. Sample volume can be largely reduced with an efficient pre-concentration process. Some approaches such as hollow-fiber ultra-filtration and electrokinetic technique have been applied to bacterial concentration. Since none of these methods can provide a concentrating method with a stable recovery efficiency, bacterial concentration still remains challenging Ceramic micro- filter can be used to concentrate the bacteria but the cross flow system keeps the bacteria in suspension. Similar harvesting bacteria using ultra-filtration showed an average recovery efficiency of 43% [1] and other studies achieved recovery rates greater than 50% [2]. In this study, an enhanced ceramic micro-filter with 0.14 μm pore size was proposed and demonstrated to optimize the concentration of E.coli. A high recovery rate (mean value >90%) and a high volumetric concentration ratio (>100) were achieved. Known quantities (104 to 106 CFU/ml) of E.coli cells were spiked to different amounts of phosphate buffered saline (0.1 to 1 L), and then concentrated to a final retentate of 5 ml to 10 ml. An average recovery efficiency of 95.3% with a standard deviation of 5.6% was achieved when the volumetric con- centration ratio was 10. No significant recovery rate loss was indicated when the volumetric concentration ratio reached up to 100. The effects of multiple parameters on E.coli recovery rate were also studied. The obtained results indicated that the optimized ceramic micro- filtration system can successfully concentrate E.coli cells in water with an average recovery rate of 90.8%.

Effect of investment type and mold temperature on casting accuracy and titanium-ceramic bond.

PubMed

Leal, Mônica Barbosa; Pagnano, Valéria Oliveira; Bezzon, Osvaldo Luiz

2013-01-01

This study evaluated the casting accuracy of crown margins and metal-ceramic shear bond strength (SBS) of pure titanium injected into casting molds made using 2 investment types at 3 mold temperatures. Sixty crown (30-degree beveled finish line) and 60 cylinder (5mm diameter × 8mm high) patterns were divided into 6 groups (n=10), and cast using a phosphate-bonded investment (P) and a magnesium oxide-bonded investment (U), at 400°C (groups P400 and U400), 550°C (groups P550 and U550) and 700°C (groups P700 and U700) mold temperatures. Crown margins were recorded in impression material, the degree of marginal rounding was measured and margin length deficiencies (µm) were calculated. Titanium-ceramic specimens were prepared using Triceram ceramic (2mm high) and SBS was tested. Failure modes were assessed by optical microscopy. Data were subjected to two-way ANOVA and Tukey's HSD test (α=0.05). For casting accuracy, expressed by marginal deficiency (µm), investment U provided more accurate results (64 ± 11) than P (81 ± 23) (p<0.001). The increase in temperature resulted in different effects for the tested investments (p<0.001), as it provided better casting accuracy for U700 (55 ± 7) and worse for P700 (109 ± 18). Casting accuracy at 700°C (82 ± 31) was significantly different from 400°C (69 ± 9) and 550°C (68 ± 9) (p<0.05). For SBS, there was no significant differences among the groups for factors investment (p=0.062) and temperature (p=0.224), or for their interaction (p=0.149). Investment U provided better casting accuracy than investment P. The SBS was similar for all combinations of investments and temperatures.

Macrosegregation Resulting from Directional Solidification Through an Abrupt Change in Cross-Sections

NASA Technical Reports Server (NTRS)

Lauer, M.; Poirier, D. R.; Ghods, M.; Tewari, S. N.; Grugel, R. N.

2017-01-01

Simulations of the directional solidification of two hypoeutectic alloys (Al-7Si alloy and Al-19Cu) and resulting macrosegregation patterns are presented. The casting geometries include abrupt changes in cross-section from a larger width of 9.5 mm to a narrower 3.2 mm width then through an expansion back to a width of 9.5 mm. The alloys were chosen as model alloys because they have similar solidification shrinkages, but the effect of Cu on changing the density of the liquid alloy is about an order of magnitude greater than that of Si. The simulations compare well with experimental castings that were directionally solidified in a graphite mold in a Bridgman furnace. In addition to the simulations of the directional solidification in graphite molds, some simulations were effected for solidification in an alumina mold. This study showed that the mold must be included in numerical simulations of directional solidification because of its effect on the temperature field and solidification. For the model alloys used for the study, the simulations clearly show the interaction of the convection field with the solidifying alloys to produce a macrosegregation pattern known as "steepling" in sections with a uniform width. Details of the complex convection- and segregation-patterns at both the contraction and expansion of the cross-sectional area are revealed by the computer simulations. The convection and solidification through the expansions suggest a possible mechanism for the formation of stray grains. The computer simulations and the experimental castings have been part of on-going ground-based research with the goal of providing necessary background for eventual experiments aboard the ISS. For casting practitioners, the results of the simulations demonstrate that computer simulations should be applied to reveal interactions between alloy solidification properties, solidification conditions, and mold geometries on macrosegregation. The simulations also presents the possibility of engineering the mold-material to avoid, or mitigate, the effects of thermosolutal convection and macrosegregation by selecting a mold material with suitable thermal properties, especially its thermal conductivity.

Stabilization and disposal of Argonne-West low-level mixed wastes in ceramicrete waste forms.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Barber, D. B.; Singh, D.; Strain, R. V.

1998-02-17

The technology of room-temperature-setting phosphate ceramics or Ceramicrete{trademark} technology, developed at Argonne National Laboratory (ANL)-East is being used to treat and dispose of low-level mixed wastes through the Department of Energy complex. During the past year, Ceramicrete{trademark} technology was implemented for field application at ANL-West. Debris wastes were treated and stabilized: (a) Hg-contaminated low-level radioactive crushed light bulbs and (b) low-level radioactive Pb-lined gloves (part of the MWIR {number_sign} AW-W002 waste stream). In addition to hazardous metals, these wastes are contaminated with low-level fission products. Initially, bench-scale waste forms with simulated and actual waste streams were fabricated by acid-base reactionsmore » between mixtures of magnesium oxide powders and an acid phosphate solution, and the wastes. Size reduction of Pb-lined plastic glove waste was accomplished by cryofractionation. The Ceramicrete{trademark} process produces dense, hard ceramic waste forms. Toxicity Characteristic Leaching Procedure (TCLP) results showed excellent stabilization of both Hg and Pb in the waste forms. The principal advantage of this technology is that immobilization of contaminants is the result of both chemical stabilization and subsequent microencapsulation of the reaction products. Based on bench-scale studies, Ceramicrete{trademark} technology has been implemented in the fabrication of 5-gal waste forms at ANL-West. Approximately 35 kg of real waste has been treated. The TCLP is being conducted on the samples from the 5-gal waste forms. It is expected that because the waste forms pass the limits set by the EPAs Universal Treatment Standard, they will be sent to a radioactive-waste disposal facility.« less

Novel resorbable glass-ceramic scaffolds for hard tissue engineering: from the parent phosphate glass to its bone-like macroporous derivatives.

PubMed

Bretcanu, Oana; Baino, Francesco; Verné, Enrica; Vitale-Brovarone, Chiara

2014-05-01

One of the major challenges of hard tissue engineering research focuses on the development of scaffolds that can match the mechanical properties of the host bone and resorb at the same rate as the bone is repaired. The aim of this work was the synthesis and characterization of a resorbable phosphate glass, as well as its application for the fabrication of three dimensional (3-D) scaffolds for bone regeneration. The glass microstructure and behaviour upon heating were analysed by X-ray diffraction, differential scanning calorimetry and hot stage microscopy. The glass solubility was investigated according to relevant ISO standards using distilled water, simulated body fluid (SBF) and Tris-HCl as testing media. The glass underwent progressive dissolution over time in all three media but the formation of a hydroxyapatite-like layer was also observed on the samples soaked in SBF and Tris-HCl, which demonstrated the bioactivity of the material. The glass powder was used to fabricate 3-D macroporous bone-like glass-ceramic scaffolds by adopting polyethylene particles as pore formers: during thermal treatment, the polymer additive was removed and the sintering of glass particles was allowed. The obtained scaffolds exhibited high porosity (87 vol.%) and compressive strength around 1.5 MPa. After soaking for 4 months in SBF, the scaffolds mass loss was 76 wt.% and the pH of the solution did not exceed the 7.55 value, thereby remaining in a physiological range. The produced scaffolds, being resorbable, bioactive, architecturally similar to trabecular bone and exhibiting interesting mechanical properties, can be proposed as promising candidates for bone repair applications.

[An experimental study on a slow-release complex with rifampicin-polylactic-co-glycolic acid-calcium 
phosphate cement].

PubMed

Wu, Jianhuang; Ding, Zhou; Lei, Qing; Li, Miao; Liang, Yan; Lu, Tao

2016-09-28

To prepare the slow-release complex with rifampicin (RFP)-polylactic-co-glycolic acid (PLGA)-calcium phosphate cement (CPC) (RFP-PLGA-CPC complex), and to study its physical and chemical properties and drug release properties in vitro.
 The emulsification-solvent evaporation method was adopted to prepare rifampicin polylactic acid-glycolic acid (RFP-PLGA) slow-release microspheres, which were divided into 3 groups: a calcium phosphate bone cement group (CPC group), a CPC embedded with RFP group (RFP-CPC group), and a PLGA slow-release microspheres carrying RFP and the self-curing CPC group (RFP- PLGA-CPC complex group). The solidification time and porosity of materials were determined. The drug release experiments in vitro were carried out to observe the compressive strength, the change of section morphology before and after drug release. 
 The CPC group showed the shortest solidification time, while the RFP-PLGA-CPC complex group had the longest one. There was statistical difference in the porosity between the CPC group and the RFP-CPC group (P<0.05); Compared to the RFP-PLGA-CPC complex group, the porosity in the CPC group and the RFP-CPC group were significantly changed (both P<0.01). There was significant difference in the compressive strength between the RFP- PLGA-CPC complex group and the CPC group (P<0.01), while there was significant difference in the compressive strength between the RFP-CPC group and the CPC group (3 days: P<0.05; 30 and 60 days: P<0.01). The change of the compressive strength in the CPC was not significant in the whole process of degradation. The sizes of PLGA microspheres were uniform, with the particle size between 100-150 μm. The microspheres were spheres or spheroids, and their surface was smooth without the attached impurities. There was no significant change in the section gap in the CPC group after soaking for 3 to 60 days. The microstructure change in the RFP-CPC group was small, and the cross section was formed by small particles. The pores of section in the RFP-PLGA-CPC complex group increased obviously, and PLGA microspheres gradually disappeared until the 60th day when there were only empty cavities left. The RFP-PLGA-CPC complex group had no obvious drugs sudden release, and the cumulative drug release rate was nearly 95% in the 60 days. The linear fitting was conducted for the drug release behavior of the complex, which was in accordance with zero order kinetics equation F=0.168×t.
 The porosity of RFP-PLGA-CPC complex is significantly higher than that of CPC, and it can keep slow release of the effective anti-tuberculosis drugs and maintain a certain mechanical strength for a long time.

On the hot cracking susceptibility of a semisolid aluminium 6061 weld: Application of a coupled solidification- thermomechanical model

NASA Astrophysics Data System (ADS)

Zareie Rajani, H. R.; Phillion, A. B.

2015-06-01

A coupled solidification-thermomechanical model is presented that investigates the hot tearing susceptibility of an aluminium 6061 semisolid weld. Two key phenomena are considered: excessive deformation of the semisolid weld, initiating a hot tear, and the ability of the semisolid weld to heal the hot tear by circulation of the molten metal. The model consists of two major modules: weld solidification and thermomechanical analysis. 1) By means of a multi-scale model of solidification, the microstructural evolution of the semisolid weld is simulated in 3D. The semisolid structure, which varies as a function of welding parameters, is composed of solidifying grains and a network of micro liquid channels. The weld solidification module is utilized to obtain the solidification shrinkage. The size of the micro liquid channels is used as an indicator to assess the healing ability of the semisolid weld. 2) Using the finite element method, the mechanical interaction between the weld pool and the base metal is simulated to capture the transient force field deforming the semisolid weld. Thermomechanical stresses and shrinkage stresses are both considered in the analysis; the solidification contractions are extracted from the weld solidification module and applied to the deformation simulation as boundary conditions. Such an analysis enables characterization of the potential for excessive deformation of the weld. The outputs of the model are used to study the effect of welding parameters including welding current and speed, and also welding constraint on the hot cracking susceptibility of an aluminium alloy 6061 semisolid weld.

Interaction of Multiple Particles with a Solidification Front: From Compacted Particle Layer to Particle Trapping.

PubMed

Saint-Michel, Brice; Georgelin, Marc; Deville, Sylvain; Pocheau, Alain

2017-06-13

The interaction of solidification fronts with objects such as particles, droplets, cells, or bubbles is a phenomenon with many natural and technological occurrences. For an object facing the front, it may yield various fates, from trapping to rejection, with large implications regarding the solidification pattern. However, whereas most situations involve multiple particles interacting with each other and the front, attention has focused almost exclusively on the interaction of a single, isolated object with the front. Here we address experimentally the interaction of multiple particles with a solidification front by performing solidification experiments of a monodisperse particle suspension in a Hele-Shaw cell with precise control of growth conditions and real-time visualization. We evidence the growth of a particle layer ahead of the front at a close-packing volume fraction, and we document its steady-state value at various solidification velocities. We then extend single-particle models to the situation of multiple particles by taking into account the additional force induced on an entering particle by viscous friction in the compacted particle layer. By a force balance model this provides an indirect measure of the repelling mean thermomolecular pressure over a particle entering the front. The presence of multiple particles is found to increase it following a reduction of the thickness of the thin liquid film that separates particles and front. We anticipate the findings reported here to provide a relevant basis to understand many complex solidification situations in geophysics, engineering, biology, or food engineering, where multiple objects interact with the front and control the resulting solidification patterns.

Powder-Metallurgy Process And Product

NASA Technical Reports Server (NTRS)

Paris, Henry G.

1988-01-01

Rapid-solidification processing yields alloys with improved properties. Study undertaken to extend favorable property combinations of I/M 2XXX alloys through recently developed technique of rapid-solidification processing using powder metallurgy(P/M). Rapid-solidification processing involves impingement of molten metal stream onto rapidly-spinning chill block or through gas medium using gas atomization technique.

Flight Planning for the International Space Station-Levitation Observation of Dendrite Evolution in Steel Ternary Alloy Rapid Solidification

NASA Technical Reports Server (NTRS)

Flemings, M. C.; Matson, D. M.; Loser, W.; Hyers, R. W.; Rogers, J. R.; Curreri, Peter A. (Technical Monitor)

2002-01-01

The paper is an overview of the status and science for the LODESTARS (Levitation Observation of Dendrite Evolution in Steel Ternary Alloy Rapid Solidification) research project. The program is aimed at understanding how melt convection influences phase selection and the evolution of rapid solidification microstructures.

Evolution of solidification texture during additive manufacturing

PubMed Central

Wei, H. L.; Mazumder, J.; DebRoy, T.

2015-01-01

Striking differences in the solidification textures of a nickel based alloy owing to changes in laser scanning pattern during additive manufacturing are examined based on theory and experimental data. Understanding and controlling texture are important because it affects mechanical and chemical properties. Solidification texture depends on the local heat flow directions and competitive grain growth in one of the six <100> preferred growth directions in face centered cubic alloys. Therefore, the heat flow directions are examined for various laser beam scanning patterns based on numerical modeling of heat transfer and fluid flow in three dimensions. Here we show that numerical modeling can not only provide a deeper understanding of the solidification growth patterns during the additive manufacturing, it also serves as a basis for customizing solidification textures which are important for properties and performance of components. PMID:26553246

Evolution of solidification texture during additive manufacturing

DOE PAGES

Wei, H. L.; Mazumder, J.; DebRoy, T.

2015-11-10

Striking differences in the solidification textures of a nickel based alloy owing to changes in laser scanning pattern during additive manufacturing are examined based on theory and experimental data. Understanding and controlling texture are important because it affects mechanical and chemical properties. Solidification texture depends on the local heat flow directions and competitive grain growth in one of the six <100> preferred growth directions in face centered cubic alloys. Furthermore, the heat flow directions are examined for various laser beam scanning patterns based on numerical modeling of heat transfer and fluid flow in three dimensions. Here we show that numericalmore » modeling can not only provide a deeper understanding of the solidification growth patterns during the additive manufacturing, it also serves as a basis for customizing solidification textures which are important for properties and performance of components.« less

Influences on Distribution of Solute Atoms in Cu-8Fe Alloy Solidification Process Under Rotating Magnetic Field

NASA Astrophysics Data System (ADS)

Zou, Jin; Zhai, Qi-Jie; Liu, Fang-Yu; Liu, Ke-Ming; Lu, De-Ping

2018-05-01

A rotating magnetic field (RMF) was applied in the solidification process of Cu-8Fe alloy. Focus on the mechanism of RMF on the solid solution Fe(Cu) atoms in Cu-8Fe alloy, the influences of RMF on solidification structure, solute distribution, and material properties were discussed. Results show that the solidification behavior of Cu-Fe alloy have influenced through the change of temperature and solute fields in the presence of an applied RMF. The Fe dendrites were refined and transformed to rosettes or spherical grains under forced convection. The solute distribution in Cu-rich phase and Fe-rich phase were changed because of the variation of the supercooling degree and the solidification rate. Further, the variation in solute distribution was impacted the strengthening mechanism and conductive mechanism of the material.